CN115321989B - Method for regulating and controlling surface roughness of ceramic substrate for LTCC and application thereof - Google Patents
Method for regulating and controlling surface roughness of ceramic substrate for LTCC and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of functional ceramics, and particularly provides a method for regulating and controlling the surface roughness of a ceramic substrate for LTCC and application thereof, wherein the method comprises the following steps: the ceramic substrate for LTCC is formed by sintering a green ceramic tape made of ceramic slurry; the glass powder in the ceramic slurry is calcium-boron-lanthanum glass; the dispersant in the ceramic slurry is a dispersant mixed solution formed by mixing an amino acid ester dispersant and a phosphate ester dispersant. According to the invention, the viscosity and the powder dispersibility of the tape-casting slurry can be controlled by adjusting the proportion and the dosage of the two dispersants in the LTCC slurry, so that the surface crystallization degree of a glass phase in the ceramic powder slurry in the sintering process is controlled, and the sintered substrate with controllable surface roughness is obtained, and the surface roughness of the sintered substrate can be adjusted in the aspects of smoothness, smoothness and roughness, so that the LTCC slurry has a wide application prospect in the technical fields of electronic ceramic elements, electronic device packaging and low-temperature co-fired ceramic molding.
Description
Technical Field
The invention relates to the technical field of functional ceramics, in particular to a method for regulating and controlling the surface roughness of a ceramic substrate for LTCC and application thereof.
Background
LTCC (low temperature co-fired ceramic), a typical multilayer circuit board technology, has excellent electrical and mechanical properties, and has become the mainstream mode of electronic element integration. With the rapid development and maturation of the LTCC technology, the LTCC technology is widely applied to aerospace, aviation, communication, military, automobiles, medical treatment and electronic products, and the application in these high-precision fields has higher and higher requirements on the diversification and reliability of the LTCC material.
The LTCC technology is based on the basic principle and features that low-temperature sintered ceramic powder is made into a dense green tape with precise thickness, required circuit patterns are made on the green tape by means of laser drilling, micropore grouting, precise conductor paste printing and other processes, a plurality of passive devices are embedded into the green tape for laminating, and finally sintering is carried out below 900 ℃ to form the LTCC passive/active integrated functional module.
After sintering, the conductor paste for LTCC printing is required to have good conductivity, solder erosion resistance, solder wettability, excellent adhesion, and the like. The substrate surface roughness affects not only the adhesion of the conductive paste but also the flatness and uniformity of the printed pattern. At present, two methods for regulating and controlling the roughness are provided, namely isostatic pressing of a green ceramic chip and grinding and polishing of a sintered substrate. Both add to the process and cost.
In view of this, the present invention is proposed.
Disclosure of Invention
The invention provides a method for regulating and controlling the surface roughness of a ceramic substrate for LTCC and application thereof, which are used for solving the defect that the surface roughness of the ceramic substrate for LTCC is single and is difficult to regulate in the prior art, widening the roughness range of the substrate and meeting the printing requirements of different electronic pastes by improving the designability of the substrate. According to the invention, the amino acid ester dispersant and the phosphate dispersant are mixed according to a certain proportion to be used as dispersant mixed liquid, so that the slurry dispersibility and the powder distribution in the sintering process are effectively controlled, and the ceramic substrate for the LTCC with controllable surface roughness is successfully prepared. The surface roughness of the sintered substrate is adjustable between smooth (Ra 0.16-0.28, rz 4-6 μm), smoother (Ra 0.28-0.39, rz 6-9 μm) and rough (Ra 0.39-0.50, rz9-12 μm).
The invention provides a method for regulating and controlling the surface roughness of a ceramic substrate for LTCC (low temperature co-fired ceramic), wherein the ceramic substrate for LTCC is formed by sintering a green ceramic tape formed by casting ceramic slurry;
the dispersant in the ceramic slurry is a dispersant mixed solution formed by mixing an amino acid ester dispersant and a phosphate ester dispersant;
the glass powder in the ceramic slurry is calcium boron lanthanum glass.
The matching of the conductor paste and the substrate is closely related to the adhesion strength, the film layer compactness and the stability of the electrical property. On one hand, the co-firing matching performance of the green ceramic and the slurry can be effectively improved by adjusting the components of the green ceramic and the slurry, on the other hand, the surface roughness of the substrate can be controlled and the adhesive force of the metal film layer can be adjusted according to the characteristics of viscosity, fineness and the like of different conductor slurries, so that the aim of improving the matching performance is fulfilled.
There are small gaps between powder particles in the casting slurry and steric hindrance is the main driving force for particle dispersion. The dispersant generates an adsorption layer with a certain thickness on the surface of the powder through an anchoring effect, according to the theory of entropy repulsion, the adsorption layers among different powders can be compressed but cannot mutually permeate, when the powders are close to each other, the solvation chain segments in the adsorption layers are compressed, the entropy is reduced, the free energy of the system is increased, and thus the entropy exclusion effect is generated. In addition, when the particle surface adsorption layer has a certain charge, the charged polymer layer can achieve the electrostatic repulsion effect through the charge carried by the charged polymer layer, and can prevent brownian-motion particles from approaching through the steric effect, so that the composite stable effect is achieved. According to the invention, from the aspect of a dispersant, a dispersant mixed solution prepared by selecting an amino acid ester dispersant and a phosphate ester dispersant is adopted, and the proportion of the dispersant in the LTCC ceramic slurry is adjusted, so that the dispersibility of inorganic powder in the ceramic slurry is effectively controlled, the surface crystallization degree in the green tape sintering process is further controlled, and the LTCC ceramic substrate with controllable surface roughness is obtained. If only the phosphate ester dispersant is adopted, the anchoring groups in the dispersant are mainly-COOH, and the anchoring groups and-OH groups on the surface of the powder particles generate hydrogen bonds through-OH-O stretching vibration, so that the powder particles absorb the hydrogen bondsAttaching the powder particles on the surface of the powder particles; in this case, the mechanism of action of the dispersant is mainly steric hindrance. Whereas if only an amino acid ester dispersant is used, the anchoring groups in the dispersant are predominantly-NH 2 So that the whole molecule presents weak cationic property, thereby forming hydrogen bonds with the surface of the powder to generate anchoring effect and achieving the purpose of steric hindrance. Different from the former two, the action mechanism of the mixed liquid dispersant provided by the invention is to combine the electrostatic repulsion and steric hindrance effects, so that the powder particles can achieve a more stable dispersion effect in the casting slurry. When the kind and the proportion of the mixed liquid dispersant reach the optimal values, the-COOH in the phosphate dispersant reacts with the-OH on the particle surface more easily to serve as the main anchoring function, and the amino acid ester dispersant is wound with the phosphate dispersant through the polymer chain entanglement function and the-NH inside the phosphate dispersant 2 The existence of the two mixed dispersants is also beneficial to the formation of hydrogen bonds between polymers, so that the two mixed dispersants macroscopically show that a charged polymer adsorption layer is formed on the surface of powder particles, the electrostatic steric hindrance effect is further stabilized and enlarged, and a better dispersion effect is achieved. However, it should be noted that the chain entanglement between the polymers can easily cause the formation of polymer clusters, so that the two dispersants lose their original dispersing effects, resulting in the occurrence of agglomeration between powder particles. Therefore, it is important to adjust the type and ratio of the dispersant in the mixed solution to obtain the optimum content.
Ceramic substrates for LTCC using glass/ceramic as a raw material can be classified into a crystallized glass/ceramic system and an amorphous glass/ceramic system. The calcium-boron-lanthanum glass belongs to crystallized glass, and has low softening point, controllable crystallization performance and good chemical stability. Compared with other glass materials, the calcium-boron-lanthanum glass is easier to separate out crystal phase in the sintering process, and finally influences the surface roughness of the sintered substrate. Therefore, the dispersion degree of the calcium boron lanthanum glass powder in the slurry is adjusted through a proper dispersant solution, and then the crystallization behavior of the glass powder in the sintering process is controlled, so that the ceramic substrate for the LTCC with different surface roughness is obtained.
According to the method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC, provided by the invention, the amino acid ester dispersant is Solsperse20000 or TEGO-700.
According to the method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC, provided by the invention, the phosphate dispersant is BYK-110, BYK-111 or BYK-22552.
The method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC comprises the following steps:
(1) Uniformly mixing an amino acid ester dispersant and a phosphate ester dispersant to obtain a dispersant mixed solution;
in the step (1), the mixing can be performed by magnetic stirring, and the stirring time is 10-40 minutes.
(2) Uniformly mixing (such as in a stirring manner) a solvent, a binder, a plasticizer and the dispersant mixed solution to obtain an organic carrier;
(3) Uniformly mixing glass powder, ceramic powder and the organic carrier (for example, in a ball milling mixing mode, the ball milling mixing time is 36-60 hours) to obtain ceramic slurry;
(4) Carrying out tape casting on the ceramic slurry to obtain a raw ceramic tape;
the step (4) may specifically be that the ceramic slurry is subjected to vacuum defoaming treatment, and then tape casting is performed to obtain the LTCC raw ceramic tape.
(5) And cutting, hot-pressing, laminating and sintering the green ceramic tape to obtain the ceramic substrate.
Hot-pressing lamination refers to laminating a plurality of layers (such as 8 layers) in thickness and then carrying out hot pressing to obtain a block;
the sintering may be performed in a sintering furnace.
According to the method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC, the mass ratio of the amino acid ester dispersant to the phosphate dispersant in the dispersant mixed solution is (25-50) to (50-75), and the mass fraction of the dispersant mixed solution is 1-4% of the total mass of the glass powder and the ceramic powder;
preferably, the mass fraction of the dispersant mixed liquid is 1.5% of the total mass of the glass powder and the ceramic powder.
In the invention, the mass fraction of the dispersant mixed liquid is controlled within a certain range. The dispersing agent is a surfactant which has two opposite properties of hydrophilicity and lipophilicity on a molecular structure, is adsorbed on the surface of powder particles and acts through an electrostatic repulsion and steric hindrance stabilization mechanism. When the dispersant is used, the dosage is strictly controlled, and if the dosage is too small, the surface of the particles cannot be completely covered, a steric hindrance mechanism is difficult to exert effect, the electrostatic repulsion effect is reduced, soft aggregates are generated, and the dispersion stability of the slurry is reduced; when the amount of the dispersant is too much, the excessive dispersant is bridged and aggregated to cause powder agglomeration, and the stability of the slurry is also reduced. The reduction of the dispersion stability of the casting slurry can cause uneven powder distribution in the casting process, thereby influencing the mechanical and electrical properties of the sintered substrate.
According to the method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC, provided by the invention, the solvent comprises at least two of ethyl acetate, butyl acetate and isopropanol;
according to the method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC, provided by the invention, the binder is polymethyl methacrylate or polybutyl methacrylate.
According to the method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC, provided by the invention, the plasticizer is dibutyl phthalate or dioctyl phthalate.
According to the method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC, provided by the invention, in the ceramic slurry, the glass powder accounts for 15-40 wt% of the ceramic slurry; the ceramic powder accounts for 30-50 wt% of the ceramic slurry; the organic carrier accounts for 15-40 wt% of the ceramic slurry.
According to the method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC, provided by the invention, the D50 of the glass powder is 1.2-2.0 microns.
According to the method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC, provided by the invention, the ceramic powder is more than one of alpha-alumina, beta-alumina and gamma-alumina, and the D50 of the ceramic powder is 1.5-2.2 microns.
According to the method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC, the casting speed is 0.3-1.0 m/min;
preferably, the casting speed is 0.5m/min to 1.0m/min.
According to the method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC, provided by the invention, the sintering temperature is 845-895 ℃, and the sintering time is 18-36 h.
The method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC is applied to the ceramic substrate for the LTCC, and the surface roughness of the ceramic substrate for the LTCC is smooth, smoother or rough;
the smooth means that Ra is 0.16-0.28, and Rz is 4-6 μm;
the smoother means that Ra is 0.28-0.39, and Rz is 6-9 μm;
the roughness means that Ra is 0.39 to 0.50 and Rz is 9 to 12 μm.
According to the method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC, provided by the invention, two specific types of dispersants are selected and mixed, and further, the proportion and the using amount of the two dispersants in the LTCC slurry are regulated, so that the viscosity and the powder dispersibility of the tape-casting slurry can be controlled, the surface crystallization degree of a glass phase in the ceramic powder slurry in the sintering process is controlled, the sintered substrate with controllable surface roughness is obtained, and the surface roughness of the sintered substrate can be regulated in a smooth, relatively smooth and rough state. The method has the advantages of low production cost, simple process and controllable reaction conditions, is suitable for regulating and controlling large-batch casting slurry, so that the sintered substrates with multiple batches of surface roughness can be obtained, and has wide application prospects in the technical fields of electronic ceramic elements, electronic device packaging and low-temperature co-fired ceramic molding.
Drawings
In order to more clearly illustrate the technical solutions of the present invention or the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, 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 photomicrograph of the surface of a substrate sintered at 850 ℃ according to examples 1, 2, 3 and 1 of the present invention; wherein (a) is example 1, (b) is example 2, (c) is example 3, and (d) is comparative example 1;
FIG. 2 is a scanning electron microscope photograph of the surface of a substrate sintered at 850 ℃ according to example 1, example 2, example 3 and comparative example 1; wherein (a) is example 1, (b) is example 2, (c) is example 3, and (d) is comparative example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The examples do not show the specific techniques or conditions, according to the technical or conditions described in the literature in the field, or according to the product specifications. The reagents or instruments used are conventional products available from regular distributors, not indicated by the manufacturer.
Solsperse20000 in the invention is sourced from Lu Borun of the United states;
TEGO-700 in the present invention is derived from Digao Chemicals;
BYK-110, BYK-111 and BYK-22552 in the present invention are derived from Bi Kehua Chemicals.
The method for controlling the surface roughness of the ceramic substrate for LTCC and the application thereof according to the present invention will be described with reference to fig. 1 to 2.
All roughness measurements mentioned in the present invention were measured by Atomic Force Microscopy (AFM).
According to the mechanical properties mentioned in the invention, a three-point bending test sample of a sintered substrate is prepared by referring to a national standard GB/T6569-2006 fine ceramic bending strength test method, the three-point bending strength test is carried out on an E42 type universal testing machine of the American MTS company, the stress surface of the test sample is grinded and polished by diamond, the test span is 15mm, the moving speed of a pressure head is 0.5mm/min, and the maximum bending strength of the test sample is obtained.
The 20GHz dielectric constant mentioned in the present invention is a dielectric constant at 20GHz of a sample measured by a network analyzer of the E5080B type resonator method of Keysight corporation, USA, and the sample size is 5mm × 4.5mm × 115 μm.
Example 1
A method for regulating and controlling the surface roughness of a ceramic substrate for LTCC comprises the following specific steps:
(1) Respectively weighing Solsperse20000 3.8g and BYK-111.2g, adding into a beaker of 50ml dried in advance, placing the beaker on a magnetic stirrer, stirring at normal temperature of 25 ℃ for 10min, and obtaining a dispersant mixed solution when no obvious suspension bead or layering phenomenon exists in the liquid in the beaker, which indicates that the stirring is finished;
(2) Respectively weighing 60g of ethyl acetate, 60g of butyl acetate, 27g of polymethyl methacrylate, 14g of dioctyl phthalate and 3g of dispersant mixed solution into a ball milling tank, adding a ball milling medium, and premixing for 4h at the normal temperature of 25 ℃ to obtain an organic carrier which is uniformly dispersed and has no undissolved particles;
(3) 100g of glass powder (D50 =1.5 μm) and 100g of alpha-alumina powder (D50 =2.0 μm) were weighed and put into a ball mill pot prepared with an organic vehicle in advance, and ball-milled at normal temperature and 25 ℃ for 36 hours to obtain ceramic slurry.
(4) And (3) carrying out vacuum defoaming treatment on the ceramic slurry, and then obtaining the LTCC green tape with the thickness of 120 microns at the casting speed of 0.8 m/min.
(5) Cutting the green porcelain tape, laminating 8 layers of the green porcelain tape, hot-pressing to obtain a block, placing the block in a sintering furnace, and heating the block to 845 ℃ in a gradient manner for 20h to obtain the substrate with the surface roughness Ra =0.21 μm and Rz =5.17 μm. The three-point bending mechanical strength of the sintered substrate was 193.17MPa, and the dielectric constant of 20GHz was 6.92.
Example 2
A method for regulating and controlling the surface roughness of a ceramic substrate for LTCC comprises the following specific steps:
(1) Respectively weighing Solsperse20000 4.5g and BYK-111-5.5g, adding into a 50ml beaker dried in advance, placing the beaker on a magnetic stirrer, stirring at the normal temperature of 25 ℃ for 10min, and obtaining a dispersant mixed solution when the stirring is finished when no obvious suspension bead and layering phenomenon exists in the liquid in the beaker;
(2) Respectively weighing 60g of ethyl acetate, 60g of butyl acetate, 27g of polymethyl methacrylate, 14g of dioctyl phthalate and 3g of dispersant mixed solution into a ball milling tank, adding a ball milling medium, and premixing for 4h at the normal temperature of 25 ℃ to obtain an organic carrier which is uniformly dispersed and has no undissolved particles;
(3) 100g of glass powder and 100g of alpha-alumina powder are weighed and added into a ball milling tank with an organic carrier prepared in advance, and ball milling is carried out for 36 hours at the normal temperature of 25 ℃ to obtain ceramic slurry.
(4) And (3) carrying out vacuum defoaming treatment on the ceramic slurry, and then obtaining the LTCC green tape with the thickness of 120 microns at the casting speed of 0.8 m/min.
(5) Cutting the green ceramic tape, laminating 8 layers of the green ceramic tape, hot-pressing to obtain a block, placing the block in a sintering furnace, and heating the block to 845 ℃ in a gradient manner for 20h to obtain the substrate with the surface roughness Ra =0.32 μm and Rz =6.86 μm. The three-point bending mechanical strength of the sintered substrate was 194.33MPa, and the dielectric constant of 20GHz was 6.87.
Example 3
A method for regulating and controlling the surface roughness of a ceramic substrate for LTCC comprises the following specific steps:
(1) Weighing Solsperse20000 3g and BYK-111 g respectively, adding into a 50ml beaker dried in advance, placing the beaker on a magnetic stirrer, stirring at normal temperature of 25 ℃ for 10min until no obvious suspension bead and layering phenomenon exist in the liquid in the beaker, and indicating that a dispersant mixed liquid is obtained after stirring is finished;
(2) Respectively weighing 60g of ethyl acetate, 60g of butyl acetate, 27g of polymethyl methacrylate, 14g of dioctyl phthalate and 3g of dispersant mixed solution into a ball milling tank, adding a ball milling medium, and premixing for 4h at the normal temperature of 25 ℃ to obtain an organic carrier which is uniformly dispersed and has no undissolved particles;
(3) 100g of glass powder and 100g of alpha-alumina powder are weighed and added into a ball milling tank with an organic carrier prepared in advance, and ball milling is carried out for 36 hours at the normal temperature of 25 ℃ to obtain ceramic slurry.
(4) And (3) carrying out vacuum defoaming treatment on the ceramic slurry, and then obtaining the LTCC green tape with the thickness of 120 microns at the casting speed of 0.8 m/min.
(5) Cutting the green porcelain tape, laminating 8 layers of the green porcelain tape, hot-pressing to obtain a block, placing the block in a sintering furnace, and heating the block to 845 ℃ in a gradient manner for 20h to obtain the substrate with the surface roughness Ra =0.45 μm and Rz =11.53 μm. The three-point bending mechanical strength of the sintered substrate is 191.86MPa, and the dielectric constant of 20GHz is 6.90.
Example 4
A method for regulating and controlling the surface roughness of a ceramic substrate for LTCC comprises the following specific steps:
(1) Respectively weighing Solsperse20000 3.5g and BYK-22552.5 g, adding into a 50ml beaker dried in advance, placing the beaker on a magnetic stirrer, stirring at normal temperature and 25 ℃ for 10min, and obtaining a dispersant mixed solution when stirring is finished when no obvious suspension bead and layering phenomenon exists in the liquid in the beaker;
(2) Respectively weighing 60g of ethyl acetate, 60g of isopropanol, 27g of polymethyl methacrylate, 14g of dibutyl phthalate and 3g of dispersing agent mixed solution into a ball milling tank, adding a ball milling medium, and premixing at the normal temperature of 25 ℃ for 4 hours to obtain an organic carrier which is uniformly dispersed and has no undissolved particles;
(3) And weighing 90g of glass powder and 110g of alpha-alumina powder, adding the glass powder and the alpha-alumina powder into a ball milling tank with an organic carrier prepared in advance, and carrying out ball milling for 36 hours at the normal temperature of 25 ℃ to obtain the ceramic slurry.
(4) And (3) carrying out vacuum defoaming treatment on the ceramic slurry, and then obtaining the LTCC green tape with the thickness of 120 microns at the casting speed of 0.8 m/min.
(5) Cutting the green porcelain tape, laminating 8 layers of the green porcelain tape, hot-pressing to obtain a block, placing the block in a sintering furnace, and heating the block in a gradient manner to 845 ℃ for 20h to obtain a sintered substrate with the surface roughness Ra =0.22 μm and Rz =4.96 μm. The sintered substrate had a three-point bending mechanical strength of 192.66MPa and a dielectric constant of 2 GHz of 6.88.
Example 5
A method for regulating and controlling the surface roughness of a ceramic substrate for LTCC comprises the following specific steps:
(1) Respectively weighing Solsperse20000 4.7g and BYK-22552.3 g, adding into a 50ml beaker dried in advance, placing the beaker on a magnetic stirrer, stirring at normal temperature of 25 ℃ for 10min, and obtaining a dispersant mixed solution when stirring is finished when no obvious suspension bead and no layering phenomenon exist in the liquid in the beaker;
(2) Respectively weighing 60g of ethyl acetate, 60g of isopropanol, 27g of polymethyl methacrylate, 14g of dibutyl phthalate and 3g of dispersant mixed solution into a ball milling tank, adding a ball milling medium, and premixing for 4 hours at the normal temperature of 25 ℃ to obtain an organic carrier which is uniformly dispersed and has no undissolved particles;
(3) Weighing 90g of glass powder and 110g of alpha-alumina powder, adding the glass powder and the alpha-alumina powder into a ball milling tank with an organic carrier prepared in advance, and carrying out ball milling for 36 hours at the normal temperature of 25 ℃ to obtain ceramic slurry.
(4) And (3) carrying out vacuum defoaming treatment on the ceramic slurry, and then obtaining the LTCC green tape with the thickness of 120 microns at the casting speed of 0.8 m/min.
(5) Cutting the green porcelain tape, laminating 8 layers of the green porcelain tape, hot-pressing to obtain a block, placing the block in a sintering furnace, and heating the block in a gradient manner to 845 ℃ for 20h to obtain a sintered substrate with the surface roughness Ra =0.31 μm and Rz =7.35 μm. The sintered substrate had a three-point bending mechanical strength of 191.47MPa and a dielectric constant of 2 GHz of 6.85.
Example 6
A method for regulating and controlling the surface roughness of a ceramic substrate for LTCC comprises the following specific steps:
(1) Respectively weighing Solsperse20000 2.8g and BYK-22552.2 g, adding the weighed Solsperse and BYK-22552.2 g into a 50ml beaker dried in advance, placing the beaker on a magnetic stirrer, stirring at normal temperature and 25 ℃ for 10min, and obtaining a dispersant mixed solution when no obvious suspension bead and layering phenomenon exists in the liquid in the beaker, which indicates that stirring is finished;
(2) Respectively weighing 60g of ethyl acetate, 60g of isopropanol, 27g of polymethyl methacrylate, 14g of dibutyl phthalate and 3g of dispersant mixed solution into a ball milling tank, adding a ball milling medium, and premixing for 4 hours at the normal temperature of 25 ℃ to obtain an organic carrier which is uniformly dispersed and has no undissolved particles;
(3) And weighing 90g of glass powder and 110g of alpha-alumina powder, adding the glass powder and the alpha-alumina powder into a ball milling tank with an organic carrier prepared in advance, and carrying out ball milling for 36 hours at the normal temperature of 25 ℃ to obtain the ceramic slurry.
(4) And (3) carrying out vacuum defoaming treatment on the ceramic slurry, and then obtaining the LTCC green tape with the thickness of 120 microns at the casting speed of 0.8 m/min.
(5) Cutting the green ceramic tape, laminating 8 layers of the green ceramic tape, hot-pressing to obtain a block, placing the block in a sintering furnace, and heating the block to 845 ℃ in a gradient manner for 20h to obtain a sintered substrate with the surface roughness Ra =0.43 μm and Rz =11.18 μm. The three-point bending mechanical strength of the sintered substrate was 196.15MPa, and the dielectric constant of 20GHz was 6.87.
Example 7
A method for regulating and controlling the surface roughness of a ceramic substrate for LTCC comprises the following specific steps:
(1) Respectively weighing TEGO-700.7g and BYK-110.3g, adding the TEGO-700.7g and BYK-110.3g into a 50ml beaker dried in advance, placing the beaker on a magnetic stirrer, stirring for 10min at the normal temperature of 25 ℃, and obtaining a dispersant mixed solution when the stirring is finished when no obvious suspension beads and layering phenomenon exist in the liquid in the beaker;
(2) Respectively weighing 60g of ethyl acetate, 60g of isopropanol, 27g of polymethyl methacrylate, 14g of dibutyl phthalate and 3g of dispersant mixed solution into a ball milling tank, adding a ball milling medium, and premixing for 4 hours at the normal temperature of 25 ℃ to obtain an organic carrier which is uniformly dispersed and has no undissolved particles;
(3) 100g of glass powder and 100g of alpha-alumina powder are weighed and added into a ball milling tank with an organic carrier prepared in advance, and ball milling is carried out for 36 hours at the normal temperature of 25 ℃ to obtain ceramic slurry.
(4) And (3) carrying out vacuum defoaming treatment on the ceramic slurry, and then obtaining the LTCC green tape with the thickness of 120 microns at the casting speed of 0.8 m/min.
(5) Cutting the green porcelain tape, stacking 8 layers of the green porcelain tape, performing hot pressing to obtain a block, placing the block in a sintering furnace, and performing gradient temperature rise to 845 ℃ for 20 hours to obtain a sintered substrate with the surface roughness Ra =0.16 μm and Rz =4.08 μm. The three-point bending mechanical strength of the sintered substrate is 192.90MPa, and the dielectric constant of 20GHz is 6.88.
Example 8
A method for regulating and controlling the surface roughness of a ceramic substrate for LTCC comprises the following specific steps:
(1) Respectively weighing TEGO-700.7g and BYK-110.3g, adding the TEGO-700.7g and BYK-110.3g into a 50ml beaker dried in advance, placing the beaker on a magnetic stirrer, stirring for 10min at the normal temperature of 25 ℃, and obtaining a dispersant mixed solution when the stirring is finished when no obvious suspension beads and layering phenomenon exist in the liquid in the beaker;
(2) Respectively weighing 60g of ethyl acetate, 60g of isopropanol, 27g of polymethyl methacrylate, 14g of dibutyl phthalate and 3g of dispersant mixed solution into a ball milling tank, adding a ball milling medium, and premixing for 4 hours at the normal temperature of 25 ℃ to obtain an organic carrier which is uniformly dispersed and has no undissolved particles;
(3) 100g of glass powder and 100g of alpha-alumina powder are weighed and added into a ball milling tank with an organic carrier prepared in advance, and ball milling is carried out for 36 hours at the normal temperature of 25 ℃ to obtain ceramic slurry.
(4) And (3) carrying out vacuum defoaming treatment on the ceramic slurry, and then obtaining the LTCC green tape with the thickness of 120 microns at the casting speed of 0.8 m/min.
(5) Cutting the green porcelain tape, laminating 8 layers of the green porcelain tape, hot-pressing to obtain a block, placing the block in a sintering furnace, and heating the block in a gradient manner to 845 ℃ for 20h to obtain a sintered substrate with the surface roughness Ra =0.34 μm and Rz =8.16 μm. The three-point bending mechanical strength of the sintered substrate was 195.48MPa, and the dielectric constant of 20GHz was 6.90.
Example 9
A method for regulating and controlling the surface roughness of a ceramic substrate for LTCC comprises the following specific steps:
(1) Respectively weighing TEGO-700.9 g and BYK-110.1 g, adding the TEGO-700.9 g and BYK-110.1 g into a 50ml beaker dried in advance, placing the beaker on a magnetic stirrer, stirring for 10min at the normal temperature of 25 ℃, and obtaining a dispersant mixed solution when the stirring is finished when no obvious suspension beads and layering phenomenon exist in the liquid in the beaker;
(2) Respectively weighing 60g of ethyl acetate, 60g of isopropanol, 27g of polymethyl methacrylate, 14g of dibutyl phthalate and 3g of dispersant mixed solution into a ball milling tank, adding a ball milling medium, and premixing for 4 hours at the normal temperature of 25 ℃ to obtain an organic carrier which is uniformly dispersed and has no undissolved particles;
(3) 100g of glass powder and 100g of alpha-alumina powder are weighed and added into a ball milling tank with an organic carrier prepared in advance, and ball milling is carried out for 36 hours at the normal temperature of 25 ℃ to obtain ceramic slurry.
(4) And (3) carrying out vacuum defoaming treatment on the ceramic slurry, and then obtaining the LTCC green tape with the thickness of 120 microns at the casting speed of 0.8 m/min.
(5) Cutting the green ceramic tape, stacking 8 layers of the green ceramic tape, hot-pressing to obtain a block, placing the block in a sintering furnace, and heating the block to 845 ℃ in a gradient manner for 20h to obtain a sintered substrate with the surface roughness Ra =0.50 μm and Rz =11.98 μm. The sintered substrate had a three-point bending mechanical strength of 193.75MPa and a dielectric constant of 20GHz of 6.91.
Comparative example 1
The preparation method of the ceramic substrate for the LTCC comprises the following steps basically as the steps of example 1, except that: in step (2) without step (1), the dispersant mixture was replaced with Solsperse20000 in equal amounts in step (2) to obtain a sintered substrate having a surface roughness of Ra =0.33 μm and Rz =7.04 μm. The three-point bending mechanical strength is 194.89MPa, and the dielectric constant of 20GHz is 6.87.
The sintered substrates of examples 1 to 3 and comparative example 1 were characterized, and as a result of observation through a microscope, the surfaces of the sintered substrates of examples 1 to 3 were in three states of smooth, smoother, and rough, respectively, and comparative example 1 was in a smoother state, as shown in fig. 1. The scanning electron microscope observation shows that the result is shown in fig. 2, and the surface of the example 1, namely fig. 1 (a), is uniformly distributed with equal large particles; in example 2, part of dendritic crystal phase is precipitated on the surface of the material shown in figure 1 (b) and is inserted among particles; the dendrites further grow on the surface of example 3, fig. 1 (c), and the number is significantly increased.
It can be seen that the surface roughness of the substrate is related to the dispersibility of the powder in the ceramic slurry, the powder dispersion state is different, the fine powder agglomeration condition is different, and further the crystallization degree of the substrate surface is different, and finally the substrate with different surface roughness is formed by sintering. Therefore, by controlling the proportion of the two dispersants, the surface roughness of the prepared sintered substrate is changed, and the purpose of controlling the surface roughness of the sintered substrate is achieved. In addition, as can be seen from the three-point bending mechanical strength and the dielectric constant of 20GHz of each example and comparative example, when the proportion of the dispersant is fixed, the kind and the internal proportion of the dispersant only change the surface roughness of the substrate, and do not affect the mechanical and electrical properties of the substrate.
Comparative example 2
A preparation method of a ceramic substrate for LTCC comprises the following specific steps:
(1) Respectively weighing 60g of ethyl acetate, 60g of isopropanol, 27g of polymethyl methacrylate, 14g of dibutyl phthalate and BYK-22552 in a ball milling tank, adding a ball milling medium, and premixing for 4 hours at the normal temperature of 25 ℃ to obtain an organic carrier which is uniformly dispersed and has no undissolved particles;
(2) And weighing 90g of glass powder and 110g of alpha-alumina powder, adding the glass powder and the alpha-alumina powder into a ball milling tank with an organic carrier prepared in advance, and carrying out ball milling for 36 hours at the normal temperature of 25 ℃ to obtain the ceramic slurry.
(3) And (3) carrying out vacuum defoaming treatment on the ceramic slurry, and then obtaining the LTCC green tape with the thickness of 120 microns at the casting speed of 0.8 m/min.
(4) Cutting the green porcelain tape, laminating 8 layers of the green porcelain tape, hot-pressing to obtain a block, placing the block in a sintering furnace, and heating the block in a gradient manner to 845 ℃ for 20h to obtain a sintered substrate with the surface roughness Ra =0.31 μm and Rz =7.42 μm. The sintered substrate had a three-point bending mechanical strength of 191.64MPa and a dielectric constant of 20GHz of 6.91.
Comparative example 3
The preparation method of the ceramic substrate for the LTCC comprises the following steps basically as the steps of example 1, except that: in step (2) without step (1), BYK-111 was substituted for the dispersant mixture in equal amounts in step (2) to obtain a sintered substrate having a surface roughness Ra =0.34 μm and Rz =7.92 μm. The three-point bending mechanical strength of the sintered substrate was 195.12MPa, and the dielectric constant of 20GHz was 6.88.
Comparative example 4
The preparation method of the ceramic substrate for the LTCC comprises the following steps basically as the steps of example 1, except that: in step (2) without step (1), the dispersant mixed solution was replaced with TEGO-700 in equal amount to obtain a sintered substrate having a surface roughness Ra =0.32 μm and an Rz =6.82 μm. The sintered substrate had a three-point bending mechanical strength of 193.96MPa and a dielectric constant of 20GHz of 6.90.
Comparative example 5
The preparation method of the ceramic substrate for the LTCC comprises the following steps basically as the steps of example 1, except that: in step (2) without step (1), the dispersant mixture was replaced with BYK-110 in an equal amount to obtain a sintered substrate having a surface roughness of Ra =0.38 μm and Rz =8.55 μm. The three-point bending mechanical strength of the sintered substrate is 191.82MPa, and the dielectric constant of 20GHz is 6.87.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (9)
1. The method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC is characterized in that the ceramic substrate for the LTCC is formed by sintering a green ceramic tape formed by casting ceramic slurry;
the dispersant in the ceramic slurry is a dispersant mixed solution formed by mixing an amino acid ester dispersant and a phosphate ester dispersant; the amino acid ester dispersant is Solsperse20000 or TEGO-700; the phosphate dispersant is BYK-110, BYK-111 or BYK-22552;
the glass powder in the ceramic slurry is calcium-boron-lanthanum glass;
the proportion and the dosage of the amino acid ester dispersant and the phosphate ester dispersant in the ceramic slurry are adjusted, the viscosity and the powder dispersibility of the tape-casting slurry can be controlled, so that the surface crystallization degree of a glass phase in the ceramic slurry in the sintering process of a ceramic substrate is controlled, and the surface roughness of the ceramic substrate is adjustable.
2. The method of modulating surface roughness of a ceramic substrate for LTCC of claim 1, comprising the steps of:
(1) Uniformly mixing an amino acid ester dispersant and a phosphate ester dispersant to obtain a dispersant mixed solution;
(2) Uniformly mixing a solvent, a binder, a plasticizer and the dispersant mixed solution to obtain an organic carrier;
(3) Uniformly mixing glass powder, ceramic powder and the organic carrier to obtain ceramic slurry;
(4) Carrying out tape casting on the ceramic slurry to obtain a raw ceramic tape;
(5) And cutting, hot-pressing, laminating and sintering the green ceramic tape to obtain the ceramic substrate.
3. The method for regulating and controlling the surface roughness of the ceramic substrate for the LTCC according to claim 2, wherein the mass ratio of the amino acid ester dispersant to the phosphate dispersant in the dispersant mixed solution is (25-50) - (50-75), and the mass fraction of the dispersant mixed solution is 1% -4% of the total mass of the glass powder and the ceramic powder.
4. The method for controlling the surface roughness of the ceramic substrate for LTCC according to claim 3, wherein the mass fraction of the dispersant mixed solution is 1.5% of the total mass of the glass powder and the ceramic powder.
5. The method of claim 2, wherein the solvent comprises at least two of ethyl acetate, butyl acetate and isopropyl alcohol.
6. The method of claim 2, wherein the binder is polymethyl methacrylate or polybutyl methacrylate.
7. The method of claim 2, wherein the plasticizer is dibutyl phthalate or dioctyl phthalate.
8. The method for controlling the surface roughness of the ceramic substrate for LTCC according to claim 2, wherein the ceramic powder is one or more of α -alumina, β -alumina and γ -alumina.
9. The method of modulating the surface roughness of a ceramic substrate for LTCC as claimed in any one of claims 1 to 8 applied to LTCC materials wherein the surface roughness of the ceramic substrate for LTCC is smooth, relatively smooth or rough;
the smooth is that Ra is 0.16 to 0.28, and Rz is 4~6 mu m;
the smoother refers to Ra of 0.28 to 0.39 and Rz of 6~9 mu m;
the roughness is that Ra is 0.39 to 0.50, and Rz is 9 to 12 μm.
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