Preparation method and printing method of embedded medium printing paste for HTCC
By introducing pore-forming agent into the HTCC medium to form a microporous structure, the problem of cracking of ceramic substrates due to poor thermal expansion adaptation at high temperature is solved, and the effective thermal expansion matching between the medium and the substrate is achieved.
Patent Information
- Application Number
- CN202311527535.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-11-16
- Publication Date
- 2025-05-16
AI Technical Summary
The existing HTCC dielectric printing paste cannot effectively adapt to the thermal expansion of the ceramic substrate at high temperatures, resulting in cracking and failure of the ceramic substrate.
By introducing a pore-forming agent, such as carbon black, into the alumina medium, a microporous structure is formed through multiple ball milling and grinding, and volume deformation caused by thermal expansion is absorbed.
It effectively solves the problem of ceramic substrate cracking due to poor thermal expansion adaptation at high temperatures. The volume deformation is absorbed through the microporous structure, and the thermal expansion matching between the medium and the substrate is improved.
Smart Images
Figure CN120004649A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of printing paste, and in particular to a preparation method and a printing method of an embedded medium printing paste for HTCC. Background Art
[0002] In recent years, with the development of HTCC technology, the temperature tolerance of active electronic components has continued to increase. For example, solid electrolyte gas sensors with embedded heaters require operating temperatures ranging from 300 to 800°C, depending on the requirements of different application scenarios. With the increase in operating temperature, the requirements for insulating media are becoming increasingly higher, especially the thermal expansion matching of the dielectric material used for electrical isolation heaters and the ceramic substrate material at high temperatures. The higher the operating temperature requirement and the greater the current of the heater, the higher the purity and thickness of the embedded insulating dielectric layer used for electrical isolation. Due to the difference in the thermal expansion coefficient of the dielectric material and the thermal expansion coefficient of the ceramic substrate material, at the continuously increasing operating temperature, the thermal expansion mismatch between the thickened dielectric and the ceramic substrate material is aggravated, and the thermal stress increases suddenly, which can easily lead to cracking and failure of the ceramic substrate.
[0003] In order to reduce the thermal expansion mismatch between the dielectric and the ceramic substrate material and reduce the internal thermal stress, a small amount of pores can be introduced into the originally dense dielectric film layer to form space compensation between the dielectric crystal particles during expansion to reduce thermal stress. The existing HTCC dielectric printing paste is usually prepared with dielectric (alumina powder) and organic carrier (binder, plasticizer, solvent, etc.). After HTCC processing, the fired dielectric layer is a dense structure that cannot absorb the volume deformation caused by thermal expansion adaptation. Summary of the invention
[0004] The purpose of the present invention is to overcome the deficiencies in the prior art, provide a preparation method and a printing method of an embedded dielectric printing slurry for HTCC, and solve the technical problem of ceramic cracking caused by thermal expansion adaptation between the embedded dielectric layer and the substrate ceramic under high temperature working in the existing dielectric slurry processing.
[0005] To achieve the above object, the present invention is implemented by adopting the following technical solutions:
[0006] In a first aspect, the present invention provides a method for preparing an embedded medium printing paste for HTCC, comprising:
[0007] According to weight percentage, 70-90% of alumina powder, 18-19% of low boiling point solvent, and 0.5-1% of dispersant are added to a ball mill, and the ball mill is used for the first ball milling dispersion;
[0008] According to weight percentage, 6-10% of a binder, 3-5% of a plasticizer, and 3-5% of a diluent are added to a ball mill, and a second ball milling dispersion is performed through the ball mill;
[0009] After the second ball milling dispersion, the mixture is placed in a defoamer for defoaming treatment, and after the defoaming treatment, the mixture is placed in a stirring container;
[0010] Add 0.5-1% of dispersant by weight to the stirring container and stir and mix;
[0011] According to the weight percentage, 8-15% of the pore-forming agent is added to the stirring container several times, and the mixture is stirred and mixed. After the mixture is stirred and mixed, the mixture is put into a ball mill, and the mixture is dispersed by ball milling for the third time in the ball mill;
[0012] After the third ball milling dispersion, the slurry is put into a rolling mill for grinding, and a degassing treatment is performed after grinding to obtain a uniform and stable slurry.
[0013] Optionally, the first ball milling dispersion lasts for 5-10 hours, the second ball milling dispersion lasts for 5-20 hours, and the third ball milling dispersion lasts for 5-20 hours.
[0014] Optionally, the pore-forming agent is carbon black.
[0015] Optionally, the rolling mill adopts a three-roll rolling mill, and grinding is performed by adjusting different roller gaps.
[0016] In a second aspect, the present invention provides a method for printing a HTCC embedded medium printing paste, comprising:
[0017] The slurry was prepared by the above-mentioned preparation method, and the viscosity was tested;
[0018] Select the mesh size and thickness of the printing screen according to the thickness requirements of the embedded medium, and then use the slurry that has passed the viscosity test for printing.
[0019] Optionally, the printing thickness is 150 μm.
[0020] Compared with the prior art, the present invention has the following beneficial effects:
[0021] The present invention provides a preparation method and printing method of an embedded dielectric printing slurry for HTCC. The preparation method comprises the following steps: preparing an alumina dielectric and an organic carrier, adding a pore-forming agent in multiple times, and forming required micropores in the alumina dielectric layer after the carbon black is completely volatilized as the temperature rises in a subsequent sintering process. The invention can effectively solve the technical problem of ceramic cracking caused by thermal expansion adaptation between the embedded dielectric layer and the substrate ceramic under high temperature working conditions in the existing dielectric slurry processing. BRIEF DESCRIPTION OF THE DRAWINGS
[0022] Figure 1 The present invention is a schematic flow chart of a method for preparing an embedded medium printing paste for HTCC provided in an embodiment of the present invention. DETAILED DESCRIPTION
[0023] The present invention will be further described below in conjunction with the accompanying drawings. The following embodiments are only used to more clearly illustrate the technical solution of the present invention, and cannot be used to limit the protection scope of the present invention.
[0024] Embodiment 1:
[0025] like Figure 1 As shown, an embodiment of the present invention provides a method for preparing an embedded medium printing paste for HTCC, comprising the following steps:
[0026] Step 1: Add 70-90% alumina powder, 18-19% low boiling point solvent and 0.5-1% dispersant into a ball mill according to weight percentage, and perform the first ball milling dispersion through the ball mill; the first ball milling dispersion lasts for 5-10 hours.
[0027] Step 2: Add 6-10% of binder, 3-5% of plasticizer and 3-5% of diluent into the ball mill according to weight percentage, and perform a second ball milling dispersion in the ball mill; the second ball milling dispersion lasts for 5-20 hours.
[0028] Step 3, after the second ball milling dispersion, put it into a defoamer for defoaming treatment, and put it into a stirring container after the defoaming treatment;
[0029] Step 4: Add 0.5-1% of dispersant by weight to the stirring container and stir and mix;
[0030] Step 5: Add 8-15% of the pore-forming agent by weight percentage to the stirring container several times, and stir and mix. After stirring and mixing, put it into a ball mill and perform a third ball milling dispersion in the ball mill; the third ball milling dispersion lasts for 5-20 hours.
[0031] In an optional embodiment, the pore former is carbon black.
[0032] Step 6: After the third ball milling dispersion, the mixture is put into a rolling mill for grinding, and degassing is performed after grinding to obtain a uniform and stable slurry.
[0033] In an optional embodiment, the rolling mill is a three-roll rolling mill, and grinding is performed by adjusting different roller gaps.
[0034] Embodiment 2:
[0035] Step S11, according to weight percentage, add 81.5% of alumina powder, 18% of low boiling point solvent, and 0.5% of dispersant into a ball mill, and perform the first ball milling dispersion in the ball mill; the first ball milling dispersion lasts for 10 hours.
[0036] Step S12, adding 6% of binder, 3% of plasticizer and 3% of diluent into the ball mill according to weight percentage, and performing a second ball milling dispersion in the ball mill; the second ball milling dispersion lasts for 20 hours.
[0037] Step S13, after the second ball milling dispersion, placing in a defoamer for defoaming treatment, and placing in a stirring container after the defoaming treatment;
[0038] Step S14, adding 0.5% of a dispersant by weight into the stirring container, and stirring and mixing;
[0039] Step S15, adding 8% carbon black by weight percentage to the stirring container in multiple times, and stirring and mixing, putting into a ball mill after stirring and mixing, and performing a third ball milling dispersion in the ball mill; the third ball milling dispersion lasts for 20 hours.
[0040] Step S16, after the third ball milling dispersion, put it into a three-roll mill for grinding, and degassing it after grinding to obtain a uniform and stable slurry 1.
[0041] Embodiment three:
[0042] Step S21, according to weight percentage, add 80% of alumina powder, 19% of low boiling point solvent, and 1% of dispersant into a ball mill, and perform the first ball milling dispersion in the ball mill; the first ball milling dispersion lasts for 10 hours.
[0043] Step S22, according to weight percentage, add 10% binder, 5% plasticizer, and 5% diluent into the ball mill, and perform a second ball milling dispersion in the ball mill; the second ball milling dispersion lasts for 20 hours.
[0044] Step S23, after the second ball milling dispersion, placing in a defoamer for defoaming treatment, and placing in a stirring container after the defoaming treatment;
[0045] Step S24, adding 1% of a dispersant by weight into the stirring container, and stirring and mixing;
[0046] Step S25, adding 15% carbon black by weight percentage to the stirring container in multiple times, and stirring and mixing, putting into a ball mill after stirring and mixing, and performing a third ball milling dispersion in the ball mill; the third ball milling dispersion lasts for 20 hours.
[0047] Step S26, after the third ball milling dispersion, put it into a three-roll mill for grinding, and perform degassing treatment after grinding to obtain a uniform and stable slurry 2.
[0048] Embodiment 4:
[0049] The present invention provides a method for printing an embedded medium printing paste for HTCC, comprising:
[0050] The slurry was prepared by the preparation method of the above embodiment, and the viscosity was tested;
[0051] The mesh size and thickness of the printing screen are selected according to the thickness requirements of the embedded medium, and then the slurry that has passed the viscosity test is used for printing; the printing thickness is 150μm.
[0052] Subsequent steps in printing include:
[0053] After drying, the ceramic membrane strips with other functional layers are isostatically pressed, sliced, and sintered. During the carbon removal process of the sintering process, the carbon black completely volatilizes at 800°C as the temperature rises, and the required micropores are formed in the alumina dielectric layer.
[0054] The present invention absorbs the volume deformation caused by thermal expansion adaptation through micropores, thereby solving the technical problem of ceramic cracking caused by thermal expansion adaptation between the embedded dielectric layer and the substrate ceramic under high-temperature operation.
[0055] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the technical principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.
Claims
1. A method for preparing an embedded medium printing paste for HTCC, characterized in that: include: According to weight percentage, 70-90% of alumina powder, 18-19% of low boiling point solvent, and 0.5-1% of dispersant are added to a ball mill, and the ball mill is used for the first ball milling dispersion; According to weight percentage, 6-10% of a binder, 3-5% of a plasticizer, and 3-5% of a diluent are added to a ball mill, and a second ball milling dispersion is performed through the ball mill; After the second ball milling dispersion, the mixture is placed in a defoamer for defoaming treatment, and after the defoaming treatment, the mixture is placed in a stirring container; Add 0.5-1% of dispersant by weight to the stirring container and stir and mix; According to the weight percentage, 8-15% of the pore-forming agent is added to the stirring container several times, and the mixture is stirred and mixed. After the mixture is stirred and mixed, the mixture is put into a ball mill, and the mixture is dispersed by ball milling for the third time in the ball mill; After the third ball milling dispersion, the slurry is put into a rolling mill for grinding, and a degassing treatment is performed after grinding to obtain a uniform and stable slurry.
2. The method for preparing the embedded medium printing paste for HTCC according to claim 1, characterized in that: The first ball milling dispersion lasts for 5-10 hours, the second ball milling dispersion lasts for 5-20 hours, and the third ball milling dispersion lasts for 5-20 hours.
3. The method for preparing the embedded medium printing paste for HTCC according to claim 1, characterized in that: The pore-forming agent is carbon black.
4. The method for preparing the embedded medium printing paste for HTCC according to claim 1, characterized in that: The rolling mill adopts a three-roll rolling mill, and grinding is performed by adjusting different roller gaps.
5. A method for printing a HTCC embedded medium printing paste, characterized in that: include: Prepare the slurry by the preparation method according to any one of claims 1 to 4, and test the viscosity; Select the mesh size and thickness of the printing screen according to the thickness requirements of the embedded medium, and then use the slurry that has passed the viscosity test for printing.
6. The method for printing the embedded medium printing paste for HTCC according to claim 5, characterized in that: The printing thickness was 150 μm.