CN113800918B - Trace in-situ carbon-induced Si3N4 heat-conducting ceramic material and preparation method thereof - Google Patents
Trace in-situ carbon-induced Si3N4 heat-conducting ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses trace in-situ carbon-induced Si 3 N 4 Method for preparing heat-conducting ceramic material from Si 3 N 4 The powder, the sintering aid and the organic matter are used as raw materials and are prepared by modification, molding, primary sintering and secondary sintering; the organic matter generates high-activity, high-uniformity and controllable trace carbon in situ at a certain temperature to realize in-situ distribution in a silicon nitride matrix, thereby achieving oxygen removal at a crystal boundary, reducing a glass phase, improving alpha → beta phase transformation rate, solving the problems of deformation and cracking of a blank, limited crystal lattice oxygen removal effect, nonuniform organization and the like caused by nonuniform distribution when the carbon is directly added, and improving Si 3 N 4 The heat conducting property and the strength of the heat conducting ceramic material.
Description
Technical Field
The invention relates to the technical field of ceramic materials, in particular to trace in-situ carbon-induced Si 3 N 4 A heat-conducting ceramic material and a preparation method thereof.
Background
The 5G communication becomes the focus of a new round of competition in information leather of various countries in the 21 st century, and has urgent needs in the fields of aerospace, traffic, energy and the like. The integrated circuit of the communication equipment is developed to high frequency, high power, miniaturization and the like, but the high frequency causes serious signal transmission loss, the high power generates large heat to easily cause instability of the circuit, and the integrated circuit bearing substrate is required to have the performances of high heat conductivity, high thermal vibration resistance, high obdurability and the like. The silicon nitride has the characteristics of high hardness, high strength, small thermal expansion coefficient and the like, is chemically inert to metal at high temperature and has high fracture toughness, and becomes an attractive substrate material for the 5G communication field. The heat-conducting property and the dielectric loss characteristic of the silicon nitride are mainly determined by compactness, glass phase content, beta phase proportion, grain size and the like, and the trace carbon can promote crystallization of the glass phase, promote alpha → beta phase to densify, reduce lattice oxygen, further improve the heat conductivity of the material and reduce the dielectric loss.
Chinese patent with application number 2020101077487 discloses high heat conduction Si 3 N 4 Ceramics and process for their preparation, using Si 3 N 4 Powder and sintering aid Mg 2 Preparation of Si from Si and C 3 N 4 Ceramics, annealed Si 3 N 4 The thermal conductivity of the ceramic is 110 W.m -1 ·K -1 The Vickers hardness is 16.2-17.8GPa, and the bending strength is 753-846MPa. The technical scheme improves Si 3 N 4 The ceramic material has mechanical property and thermal conductivity, but the carbon is easily distributed unevenly when being directly added, and the excessive addition can reduce the compactness and increase the loss value. Therefore, how to regulate the content and the uniform distribution of the trace carbon is one of the key points for realizing the high-frequency, low-loss, high-heat conduction and the commercialization of the silicon nitride.
Disclosure of Invention
The invention aims to provide trace in-situ carbon-induced Si aiming at the defects in the prior art 3 N 4 The preparation method of the heat-conducting ceramic material realizes Si by generating trace in-situ carbon in a ceramic blank 3 N 4 High length-diameter ratio, high beta-Si of heat-conducting ceramic material 3 N 4 Phase content and high densification.
Another object of the present invention is to provide Si obtained by the above-mentioned production method 3 N 4 A thermally conductive ceramic material.
The purpose of the invention is realized by the following technical scheme:
trace in-situ carbon induced Si 3 N 4 The preparation method of the heat-conducting ceramic material comprises the following steps:
s1, modification: mixing Si 3 N 4 The powder is in acidAcid washing in the solution, removing impurity oxides, ball milling, aging and drying together with a sintering aid in an alkaline solution to obtain the modified Si 3 N 4 And sintering aid mixed powder;
s2, forming: adding organic matters into the mixed powder obtained in the step S1, uniformly mixing, and then forming the mixture to obtain a blank;
s3, primary sintering: sintering the blank at 200-1000 ℃ to degrease the blank and generate trace in-situ activated carbon;
s4, secondary sintering: carrying out hot-pressing sintering on the green body treated in the step S3 at 1700-1900 ℃, and realizing high length-diameter ratio and high beta-Si through trace in-situ activated carbon 3 N 4 Phase content and high densification to obtain Si 3 N 4 A thermally conductive ceramic material.
Further, the acidic solution in step S1 comprises HNO 3 、HCl、H 2 SO 4 One or more of acetic acid, and the concentration of the acid solution is 2-5%.
Further, the alkaline solution in step S1 includes NaOH, KOH, and ammonia water, and the concentration of the alkaline solution is 3 to 8%.
Further, the amount of the organic substance used in step S2 is 2 to 8wt%, and the organic substance includes one or more of polyethylene glycol, rubber, polyethylene, polypropylene, polyvinyl alcohol, polyester, polyamide, polyacrylonitrile, and the like.
Further, the molding process in step S2 is any one of extrusion molding, compression molding, or isostatic pressing.
Further, the step S3 includes a heat preservation process.
Further, the heat preservation process in the step S3 is at least twice.
Further, the content of the in-situ activated carbon generated in the step S3 is 0.1 to 1.0%.
Further, the pressure at the time of the secondary sintering in step S4 is 5 to 10MPa.
Si obtained by the preparation method 3 N 4 A thermally conductive ceramic material.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, through impurity removal and activation treatment of raw materials, oxides influencing the heat conductivity of the materials in the original powder can be effectively removed, the surface energy and sintering activity of the powder can be improved, the material cost can be reduced, and the acid and alkali are further neutralized to reduce environmental pollution.
The invention realizes the in-situ distribution in the silicon nitride matrix by utilizing the characteristics of high activity, high uniformity, adjustability and the like of in-situ trace carbon of an organic matter at high temperature, thereby achieving the purposes of removing oxygen at a crystal boundary, reducing a glass phase, improving the alpha → beta phase transformation rate, and reducing the problems of deformation and cracking of a blank body, limited crystal lattice oxygen removal effect, uneven tissue and the like caused by uneven distribution of directly added carbon.
The method can effectively improve the heat-conducting property and the strength of the material, and the prepared Si 3 N 4 The density of the heat-conducting ceramic material is more than 98.5%, crystal grains are fibrous, the length-diameter ratio is more than 5, and the heat conductivity coefficient reaches 130-160 W.m. -1 ·K -1 The fracture toughness reaches 7-9 MPa.m 1/2 The above.
Detailed Description
In order to facilitate understanding of the present invention, the present invention will be described in more detail with reference to the following examples, but the scope of the present invention is not limited to the following specific examples.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
This example provides a trace in situ carbon induced Si 3 N 4 The preparation method of the heat-conducting ceramic material specifically comprises the following steps:
s1, modification: mixing Si 3 N 4 Pickling the powder in an acidic solution at a concentration of 3% HNO 3 And hcl at a concentration of 3% as formulated in 1 2 O 3 And 5wt% MgO) in an alkaline solution of 5% NaOH solution, and finally washing the powder with deionized water and drying to obtain modified Si 3 N 4 And a sintering aid mixed powder;
s2, forming: adding organic matters into the mixed powder obtained in the step S1, and uniformly mixing, wherein the dosage of the organic matters is (relative to Si) 3 N 4 Powder quality) 4wt%, the organic matter is prepared by uniformly stirring 1wt% of polyethylene glycol, 1.5wt% of polyvinyl alcohol, 1wt% of polyester and 0.5wt% of polyamide according to the mass ratio; then, carrying out isostatic pressing on the mixture to obtain a blank;
s3, primary sintering: putting the blank body into a sintering furnace, heating at the speed of 3 ℃/min, and respectively preserving heat at 400 ℃ and 700 ℃ for 2 hours for pyrolysis to degrease the blank body and generate trace in-situ activated carbon, wherein the content of the in-situ activated carbon is 0.6wt%;
s4, secondary sintering: carrying out hot-pressing sintering on the blank treated in the step S3 at 1750 ℃ for 2h under the pressure of 10MPa to obtain Si 3 N 4 A thermally conductive ceramic material.
Example 2
This example provides a trace in situ carbon induced Si 3 N 4 The preparation method of the heat-conducting ceramic material specifically comprises the following steps:
s1, modification: mixing Si 3 N 4 Pickling the powder in an acidic solution at a concentration of 4% HNO 3 Solution, then mixing the settled powder with a sintering aid (3 wt% Y) 2 O 3 And 5wt% of MgO) in an alkaline solution having a concentration of 8% by weight of NH 4 OH solution, finally washing the powder by deionized water and drying to obtain modified Si 3 N 4 And a sintering aid mixed powder;
s2, forming: adding organic matters into the mixed powder obtained in the step S1, and uniformly mixing, wherein the organic matters are usedAmount (relative to Si) 3 N 4 Powder mass) of 5% by weight, the organic matter was made of 1.5% by weight of polyethylene glycol, 1% by weight of polyacrylonitrile, 2.5% by weight of polyvinyl alcohol, stirred uniformly in mass ratio; then, carrying out isostatic pressing on the mixture through a soft film sheath to obtain a blank;
s3, primary sintering: putting the blank body into a sintering furnace, heating at the speed of 3 ℃/min, and respectively preserving heat for 2 hours at 350 ℃, 520 ℃ and 750 ℃ for pyrolysis to degrease the blank body and generate trace in-situ activated carbon, wherein the content of the in-situ activated carbon is 0.8wt%;
s4, secondary sintering: carrying out hot-pressing sintering on the green body treated in the step S3 at 1890 ℃ for 2h and under the pressure of 8MPa to obtain Si 3 N 4 A thermally conductive ceramic material.
Example 3
This example provides a trace in situ carbon induced Si 3 N 4 The preparation method of the heat-conducting ceramic material specifically comprises the following steps:
s1, modification: mixing Si 3 N 4 Pickling the powder in an acidic solution at a concentration of 4% HNO 3 And hcl at a concentration of 3% was prepared in a 1 2 O 3 And 5wt% MgO) in an alkaline solution of 4% NaOH, and drying the powder after washing with deionized water to obtain modified Si 3 N 4 And sintering aid mixed powder;
s2, forming: adding organic matters into the mixed powder obtained in the step S1, and uniformly mixing, wherein the dosage of the organic matters (relative to Si) is 3 N 4 Powder mass) of 5% by weight, the organic matter was made of 1.2% by weight of polyethylene glycol, 1.5% by weight of polyethylene, 1.3% by weight of polyamide, uniformly stirred in mass ratio; then, carrying out isostatic pressing on the mixture to obtain a blank;
s3, primary sintering: putting the blank into a sintering furnace, heating at the speed of 3 ℃/min, and respectively preserving heat for 2 hours at 300 ℃, 600 ℃ and 850 ℃ for pyrolysis to degrease the blank and generate trace in-situ activated carbon, wherein the content of the in-situ activated carbon is 0.7wt%;
s4, secondary sintering: carrying out hot-pressing sintering on the blank treated in the step S3 at 1900 ℃ for 2h under the pressure of 10MPa to obtain Si 3 N 4 A thermally conductive ceramic material.
Example 4
S1, modification: mixing Si 3 N 4 The powder was pickled in an acidic solution at a concentration of 3% HCl, and the precipitated powder was mixed with a sintering aid (3 wt% Y) 2 O 3 And 5wt% of MgO) in an alkaline solution of an aqueous ammonia solution having a concentration of 4%, and finally washing the powder with deionized water and drying to obtain modified Si 3 N 4 And sintering aid mixed powder;
s2, forming: adding organic matters into the mixed powder obtained in the step S1, and uniformly mixing, wherein the dosage of the organic matters is (relative to Si) 3 N 4 Powder mass) of 6wt%, the organic matter was made of 2.5wt% polypropylene, 2.5wt% polyvinyl alcohol, 1wt% polyester by mass ratio and stirred uniformly; then, carrying out isostatic pressing on the mixture to obtain a blank;
s3, primary sintering: putting the blank body into a sintering furnace, heating at the speed of 3 ℃/min, and respectively preserving heat for 2 hours at 400 ℃, 700 ℃ and 900 ℃ for pyrolysis to degrease the blank body and generate trace in-situ activated carbon, wherein the content of the in-situ activated carbon is 0.4wt%;
s4, secondary sintering: carrying out hot-pressing sintering on the blank treated in the step S3 at 1900 ℃ for 2h and the pressure of 10MPa to obtain Si 3 N 4 A thermally conductive ceramic material.
For Si prepared in examples 1 to 4 3 N 4 The heat-conducting ceramic material is subjected to performance test, and the results are as follows:
it should be understood that the above examples are only for clearly illustrating the technical solutions of the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (6)
1. Trace in-situ carbon-induced Si 3 N 4 The preparation method of the heat-conducting ceramic material is characterized by comprising the following steps of:
s1, modification: mixing Si 3 N 4 Acid washing the powder in acid solution to remove impurity oxide, ball milling, aging and drying the powder in alkaline solution together with sintering aid to obtain modified Si 3 N 4 And sintering aid mixed powder;
s2, forming: adding an organic matter into the mixed powder obtained in the step S1, uniformly mixing, and then forming the mixture to obtain a blank;
s3, primary sintering: sintering the blank at 200-1000 ℃ to degrease the blank and generate trace in-situ activated carbon;
s4, secondary sintering: carrying out hot-pressing sintering on the green body treated in the step S3 at 1700-1900 ℃, and realizing high length-diameter ratio and high beta-Si through trace in-situ activated carbon 3 N 4 Phase content and high densification to obtain Si 3 N 4 A thermally conductive ceramic material;
the dosage of the organic matter in the step S2 is Si 3 N 4 2-8% of the powder, wherein the organic matter comprises one or more of polyethylene glycol, polyethylene, polypropylene, polyvinyl alcohol, polyester, polyamide and polyacrylonitrile;
the step S3 also comprises at least two heat preservation processes, wherein the heat preservation temperature is 400 ℃ and 700 ℃, or 350 ℃, 520 ℃ and 750 ℃, or 300 ℃, 600 ℃ and 850 ℃, or 400 ℃, 700 ℃ and 900 ℃;
the content of the in-situ activated carbon generated in the step S3 is 0.1-1.0%.
2. The trace in situ carbon induced Si according to claim 1 3 N 4 The preparation method of the heat-conducting ceramic material is characterized in that the acidic solution in the step S1 comprises HNO 3 、HCl、H 2 SO 4 And one or more of acetic acid, wherein the concentration of the acid solution is 2-5%.
3. The trace in situ carbon induced Si according to claim 1 3 N 4 The preparation method of the heat-conducting ceramic material is characterized in that the alkaline solution in the step S1 comprises NaOH, KOH and ammonia water, and the concentration of the alkaline solution is 3-8%.
4. The trace in situ carbon induced Si according to claim 1 3 N 4 The preparation method of the heat-conducting ceramic material is characterized in that the forming process in the step S2 is any one of extrusion forming, compression molding or isostatic pressing.
5. The trace in situ carbon induced Si according to claim 1 3 N 4 The preparation method of the heat-conducting ceramic material is characterized in that the pressure in the secondary sintering in the step S4 is 5-10 MPa.
6. Si obtained by the production method according to any one of claims 1 to 5 3 N 4 A thermally conductive ceramic material.
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| CN110395989A (en) * | 2019-07-25 | 2019-11-01 | 国网河南省电力公司方城县供电公司 | A kind of silicon nitride circuit baseplate material and preparation method thereof |
| CN111170745A (en) * | 2020-01-09 | 2020-05-19 | 北京科技大学 | Preparation method of high-thermal-conductivity silicon nitride substrate |
| CN111875387A (en) * | 2020-06-24 | 2020-11-03 | 广东工业大学 | Method for preparing silicon nitride ceramic with low oxygen content and high thermal conductivity by coating carbon and application thereof |
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