Photocureable silicon nitride ceramic paste and preparation method thereof

Abstract

The invention discloses a photocureable silicon nitride ceramic paste and a preparation method thereof. According to the invention, stearic acid powder and a premixed solution are additionally used asraw materials on the basis of ceramic powder, wherein the premixed solution is composed of a plurality of substances. According to the invention, through addition of the stearic acid powder, the compatibility of the ceramic powder and subsequent resin can be improved, and the solid phase content of silicon nitride ceramic can be easily improved; through optimized selection of all substances in the premixed solution, resin with high refractive index can be introduced into a resin system to reduce the difference of refractive indexes of the ceramic powder and the resin, so the single-layer curing depth of a ceramic paste can be improved; in addition, rigid group containing epoxy resin, isobornyl methacrylate (IBOMA) and the like are added into the resin to reduce shrinkage generated in theprocess of curing; and through optimization of the varieties of all substances, the photocureable ceramic paste provided by the invention has the following advantages: the solid phase content and single-layer curing depth of the isobornyl methacrylate are improved, and the shrinkage amount of the paste photocured into ceramic is reduced.

Description

Technical field

[0001] The invention belongs to the technical field of silicon nitride ceramic preparation, and in particular relates to a light-cured silicon nitride ceramic paste and a preparation method thereof.

Background technique

[0002] Nitride ceramic materials are a class of materials that can realize the integration of structure and function. They have excellent properties in mechanics, chemistry, electricity, and heat. In the field of heat-resistant and high-temperature resistant structural materials, oxide ceramics and cermets cannot be replaced. It has a wide range of applications in metallurgy, aviation, chemical industry, ceramics, electronics, machinery and semiconductor industries. With the development of science and technology, the application fields and usage requirements of silicon nitride ceramics are becoming more and more stringent. At present, the traditional manufacturing method is to form the silicon nitride powder by compression molding, or p...

Examples

preparation example Construction

[0029] The present invention will be further described in detail below in conjunction with the accompanying drawings. The present invention discloses a light-cured silicon nitride ceramic paste and a preparation method thereof. The preparation method of the ceramic specifically includes the following steps:

[0030] Step 1, mix Si 3 N 4 Powder and sintering aid form ceramic powder, in which Si 3 N 4 The powder is used as the matrix, the mass proportion is 70-90%, the balance is the sintering aid, and the mass percentage of the two is 100%; the sintering aid includes Y 2 o 3 Powder, Al 2 o 3 Powder, SiO 2 Powder, any one of them or a mixture of several, when it is a mixture, the mixing ratio is any ratio; the mixing of the entire ceramic powder adopts particle grading, and 0.5μm Si 3 N 4 Powder, 3.5μm Si 3 N 4 Powder and 0.5μm sintering aid constitute ceramic powder, among which, 3.5μm Si 3 N 4The powder accounts for 70-75% of the mass of the ceramic powder, and the...

Embodiment 1

[0035] Mixed Si 3 N 4 powder and sintering aid to form ceramic powder, Si 3 N 4 The mass proportion of powder is 73%, Y 2 o 3 Powder mass fraction is 5%, Al 2 o 3 Powder mass fraction is 3%, SiO 2 The mass fraction of the powder is 19%; the Si of 3.5μm 3 N 4 Powder mass fraction is 70%, 0.5μm Si 3 N 4 The mass fraction of the powder is 3%, and the balance is 0.5 μm of sintering aid, and stearic acid powder of 3% of the mass of the ceramic powder is added to the mass of the ceramic powder to form a ceramic mixed powder; according to the mass ratio of 0.96:2.25:1.74: 0.87:0.87:1.31:10:7.16 Mix polyurethane, bisphenol A, HDDA, IBOMA, DPHA, TPGDA and TMPTA mixed solution and high refractive index resin to form mixture A, add the photoinitiator TPO of mixture A quality 5%, pass Mix with a homogenizer to obtain a premix; add the ceramic mixed powder and dispersant to the premix, the quality of the premix is ​​40% of the mass of the ceramic mixed powder, the amount of Tego...

Embodiment 2

[0040] Step 2, paste preparation

[0041] Mixed Si 3 N 4 powder and sintering aid to form ceramic powder, Si 3 N 4 The mass proportion of powder is 75%, Y 2 o 3 Powder mass fraction is 8%, Al 2 o 3 Powder mass fraction is 6%, SiO 2 The mass fraction of the powder is 11%; the Si of 3.5μm 3 N 4 Powder mass fraction is 72%, 0.5μm Si 3 N 4 The mass fraction of the powder is 3%, and the balance is 0.5 μm of sintering aid, and stearic acid powder of 6% of the mass of the ceramic powder is added to the mass of the ceramic powder to form a ceramic mixed powder; according to the mass ratio of 0.93:2.3:1.85: 0.9:0.7:1.2:10:7.3 Mix polyurethane, bisphenol A, HDDA, IBOMA, DPHA, TPGDA and TMPTA mixed solution and high refractive index resin to form mixture A, add 6% photoinitiator TPO of mixture A quality, pass Mix with a homogenizer to obtain a premixed solution; add ceramic mixed powder and dispersant to the premixed solution, the quality of the premixed solution is 35% of th...

Technical field

[0001] The invention belongs to the technical field of silicon nitride ceramic preparation, and in particular relates to a light-cured silicon nitride ceramic paste and a preparation method thereof.

Background technique

[0002] Nitride ceramic materials are a class of materials that can realize the integration of structure and function. They have excellent properties in mechanics, chemistry, electricity, and heat. In the field of heat-resistant and high-temperature resistant structural materials, oxide ceramics and cermets cannot be replaced. It has a wide range of applications in metallurgy, aviation, chemical industry, ceramics, electronics, machinery and semiconductor industries. With the development of science and technology, the application fields and usage requirements of silicon nitride ceramics are becoming more and more stringent. At present, the traditional manufacturing method is to form the silicon nitride powder by compression molding, or p...

Examples

preparation example Construction

[0029] The present invention will be further described in detail below in conjunction with the accompanying drawings. The present invention discloses a light-cured silicon nitride ceramic paste and a preparation method thereof. The preparation method of the ceramic specifically includes the following steps:

[0030] Step 1, mix Si 3 N 4 Powder and sintering aid form ceramic powder, in which Si 3 N 4 The powder is used as the matrix, the mass proportion is 70-90%, the balance is the sintering aid, and the mass percentage of the two is 100%; the sintering aid includes Y 2 o 3 Powder, Al 2 o 3 Powder, SiO 2 Powder, any one of them or a mixture of several, when it is a mixture, the mixing ratio is any ratio; the mixing of the entire ceramic powder adopts particle grading, and 0.5μm Si 3 N 4 Powder, 3.5μm Si 3 N 4 Powder and 0.5μm sintering aid constitute ceramic powder, among which, 3.5μm Si 3 N 4The powder accounts for 70-75% of the mass of the ceramic powder, and the...

Embodiment 1

[0035] Mixed Si 3 N 4 powder and sintering aid to form ceramic powder, Si 3 N 4 The mass proportion of powder is 73%, Y 2 o 3 Powder mass fraction is 5%, Al 2 o 3 Powder mass fraction is 3%, SiO 2 The mass fraction of the powder is 19%; the Si of 3.5μm 3 N 4 Powder mass fraction is 70%, 0.5μm Si 3 N 4 The mass fraction of the powder is 3%, and the balance is 0.5 μm of sintering aid, and stearic acid powder of 3% of the mass of the ceramic powder is added to the mass of the ceramic powder to form a ceramic mixed powder; according to the mass ratio of 0.96:2.25:1.74: 0.87:0.87:1.31:10:7.16 Mix polyurethane, bisphenol A, HDDA, IBOMA, DPHA, TPGDA and TMPTA mixed solution and high refractive index resin to form mixture A, add the photoinitiator TPO of mixture A quality 5%, pass Mix with a homogenizer to obtain a premix; add the ceramic mixed powder and dispersant to the premix, the quality of the premix is ​​40% of the mass of the ceramic mixed powder, the amount of Tego...

Embodiment 2

[0040] Step 2, paste preparation

[0041] Mixed Si 3 N 4 powder and sintering aid to form ceramic powder, Si 3 N 4 The mass proportion of powder is 75%, Y 2 o 3 Powder mass fraction is 8%, Al 2 o 3 Powder mass fraction is 6%, SiO 2 The mass fraction of the powder is 11%; the Si of 3.5μm 3 N 4 Powder mass fraction is 72%, 0.5μm Si 3 N 4 The mass fraction of the powder is 3%, and the balance is 0.5 μm of sintering aid, and stearic acid powder of 6% of the mass of the ceramic powder is added to the mass of the ceramic powder to form a ceramic mixed powder; according to the mass ratio of 0.93:2.3:1.85: 0.9:0.7:1.2:10:7.3 Mix polyurethane, bisphenol A, HDDA, IBOMA, DPHA, TPGDA and TMPTA mixed solution and high refractive index resin to form mixture A, add 6% photoinitiator TPO of mixture A quality, pass Mix with a homogenizer to obtain a premixed solution; add ceramic mixed powder and dispersant to the premixed solution, the quality of the premixed solution is 35% of th...

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