CN115536399A - Full aluminum nitride ceramic heating structure device and preparation method thereof - Google Patents
Full aluminum nitride ceramic heating structure device and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a full aluminum nitride ceramic heating structure device and a preparation method thereof. Comprises an aluminum nitride conductor and an aluminum nitride insulating ceramic coating the aluminum nitride conductor. The aluminum nitride insulating ceramic forms insulation protection for the aluminum nitride conductor, the aluminum nitride conductor is subjected to graphical design and is co-sintered with the aluminum nitride insulating ceramic into a whole, and the aluminum nitride conductor and the aluminum nitride insulating ceramic are mutually fused, hot-pressed and sintered into a whole. The high-power semiconductor heating device has the excellent characteristics of low heat capacity, low energy consumption, high thermal radiation coefficient, high electric heating efficiency, small thermal expansion coefficient, no deformation at high temperature, light weight, high power, energy conservation, no pollution, safety, reliability and the like, and can meet the technical requirements on heating structure devices in modern semiconductor manufacturing technological innovation.
Description
The technical field is as follows:
the invention belongs to the technical field of aluminum nitride ceramics, and particularly relates to a full aluminum nitride ceramic heating structure device and a preparation method thereof.
Background art:
aluminum Nitride Ceramic (aluminum Nitride Ceramic) is a novel Ceramic material with excellent comprehensive performance, is an ideal material for manufacturing a new-generation semiconductor and packaging an electronic device, and has excellent performance: the aluminum nitride ceramic material has high thermal conductivity (theoretical thermal conductivity of 320W/m.k), high electrical insulation, low dielectric constant and loss, no toxicity and thermal expansion coefficient matched with silicon, is continuously developed in the directions of high integration, high speed, miniaturization and intellectualization along with semiconductor manufacturing, electronic information and power electronic technology, is widely applied to large-scale integrated circuit (LSI) manufacturing processes, and is more widely applied and developed to aluminum nitride ceramic materials.
Besides perfect heat conduction, aluminum nitride also has remarkable fluorine-oxygen corrosion resistance, excellent thermal shock resistance, durability, uniform heat distribution and the like, so that the aluminum nitride is widely applied to semiconductor process. With the innovation of large-scale integrated circuit equipment and semiconductor manufacturing technology, aluminum nitride materials have excellent chucking and de-chucking response and uniform temperature heat distribution, and equipment using aluminum nitride ceramic electrostatic chucks (ESCs) and heating plates are more and more in variety, such as ion implantation, dry etching, wafer detection and the like, which are necessary materials in the technological processes of semiconductor CVD, PECVD and the like, and particularly in the aluminum nitride ceramic electrostatic chucks and heating devices, what conductor materials are adopted to electrify the aluminum nitride carrier is more and more important.
The current processes for manufacturing aluminum nitride ceramic heating devices include the following steps: a tungsten paste thick film high temperature co-firing process (HTCC); burying tungsten filaments in the aluminum nitride; the heating circuit is thick film printed on the surface of the aluminum nitride. The traditional metal conductor heating body in the process has the following defects: 1. metals have high electrical resistance density and high thermal capacity, requiring high power. 2. The metal resistor and the insulating ceramic are co-fired, so that the metal resistor and the insulating ceramic have large dielectric loss, nonuniform heating and short service life. 3. The metal resistor and the insulating ceramic can not be uniformly sintered, and the insulating ceramic is easy to crack in the using process. 4. The electric heating efficiency is low, when the temperature is high, the resistance is increased, the power is reduced, and the power consumption is large. 5. The built-in metal resistor of the insulating structure ceramic is difficult to ensure temperature uniformity, has large temperature difference at the same temperature and is difficult to use in scenes with high temperature difference precision requirements, such as semiconductor manufacturing, special industrial heating scenes and the like.
How to enable the aluminum nitride blank and the conductive blank to be mutually interwoven and mutually infiltrated and better mutually fused at interfaces made of different materials, so that the aluminum nitride ceramic heating device can meet the technical requirements on heating structure devices in the technological innovation of modern semiconductor manufacturing, and is a problem to be solved.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
The invention content is as follows:
the invention aims to provide a full aluminum nitride ceramic heating structure device and a preparation method thereof, thereby overcoming the defects in the prior art.
In order to realize the purpose, the invention provides a preparation method of a full aluminum nitride ceramic heating structure device, which comprises the following steps:
s01: mixing 94-99 wt% of aluminum nitride powder, 1-6 wt% of sintering aid, organic solvent, binder and dispersant by a ball mill to obtain first mixed slurry;
s02: carrying out centrifugal atomization granulation on the first mixed slurry to obtain first powder with a certain sphericity;
s03: mixing 57-89 wt% of aluminum nitride powder, 10-40 wt% of metal powder, 1-3 wt% of sintering aid, organic solvent, binder and dispersant by a ball mill to obtain second mixed slurry;
s04: carrying out vacuum defoaming treatment on the second mixed slurry to obtain a mixture, carrying out post-treatment on the mixture, and carrying out crushing and granulation processes to obtain second powder with a certain sphericity;
s05: pressing and molding the second powder to prepare a first biscuit with a certain shape and size;
s06: placing the first biscuit in a glue discharging furnace for glue discharging treatment to discharge organic matters in the first biscuit, thereby obtaining a ceramic biscuit without residual carbon;
s07: placing the ceramic biscuit subjected to binder removal in a high-temperature furnace, and firing at high temperature in a nitrogen atmosphere to obtain a co-crystallized aluminum nitride-based conductive ceramic material;
s08: the first powder is pressed and formed to form a bottom layer, the aluminum nitride-based conductive ceramic material is fixed in the bottom layer through pressing, then the aluminum nitride-based conductive ceramic material is coated by the first powder to form a sandwich structure, and the sandwich structure is pressed and formed to obtain a second biscuit;
s09: and placing the second blank in a high-temperature furnace, and firing at high temperature in a nitrogen atmosphere to obtain the eutectic full aluminum nitride ceramic heating structure device.
Preferably, in the technical scheme, the aluminum nitride powder is carbon reduction method powder or powder generated by a direct nitriding method; the metal powder is Ti, mo, ta, W, ni, co, dy 2 O 3 Any one or any mixture of several of them in any ratio; the combustion assistant agent is Y 2 O 3 、CaO、Li 2 O、YF 3 And CaF 2 Any one or a mixture of any several of them in any proportion.
Preferably, in the technical scheme, the organic auxiliary agent comprises an organic solvent, a binder and a dispersant, wherein the organic solvent is butanone and/or absolute ethyl alcohol, the binder is polyvinyl butyral (PVB), and the dispersant is any one or a mixture of any several of fish oil, castor oil or Glycerol Trioleate (GTO) mixed in any proportion.
Preferably, in the technical scheme, the proportion of the sintering aid in the step S01 is not more than 7% of the total mass of the powder.
Preferably, in the technical scheme, in the step S01, the slurry with a certain viscosity and good fluidity is mixed by a ball mill in a wet ball milling manner, and the wet ball milling time is generally 5 to 20 hours.
Preferably, in the technical scheme, the first mixed slurry in the step S02 is placed into a spray granulation tower, and centrifugal atomization granulation is performed at the inlet temperature of the spray granulation tower of 150-200 ℃ to form powder balls with a certain sphericity.
Preferably, in the technical scheme, the proportion of the sintering aid in the step S03 accounts for no more than 7% of the total mass of the powder, and the proportion of the metal powder accounts for 10% -40% of the total mass of the powder.
Preferably, in the technical scheme, in the step S03, the slurry is mixed into uniform slurry with a certain viscosity and good fluidity by a wet ball milling method in a ball mill, and the wet ball milling time is generally 10 to 30 hours.
Preferably, in the technical scheme, the mixture subjected to vacuum defoaming treatment in the step S04 is placed in a high-vacuum drying device for drying treatment, the temperature of a heater is set to be less than or equal to 150 ℃, and the vacuum degree is set to be less than or equal to 0.01Mpa.
Preferably, in the technical scheme, in step S04, the crushed and granulated powder is sieved to prepare a second powder with a certain sphericity, and the particle size of the second powder is 60-200 meshes.
Preferably, in the technical scheme, the glue discharging treatment is carried out in the nitrogen atmosphere at the temperature of less than or equal to 800 ℃ in the step S06.
Preferably, in the technical scheme, in the step S07, according to different ceramic formulations, high-temperature sintering is performed in a graphite sintering furnace or a metal vacuum sintering furnace at 1600 ℃ -1860 ℃ in a nitrogen atmosphere for 4-6 hours, so as to obtain the eutectic aluminum nitride-based conductive ceramic material.
Preferably, in the technical scheme, the aluminum nitride-based conductive ceramic material is subjected to processing of a corresponding pattern before step S08, after the aluminum nitride-based conductive ceramic material is subjected to coarse grinding, cutting and slicing and conductive pattern processing, resistance of the aluminum nitride-based conductive ceramic material is tested in a partition mode according to the designed resistance, and then micro polishing is performed according to the actual resistance, so that the resistance of the conductive patterns in all the areas is ensured to be consistent.
Preferably, in the technical scheme, in the step S09, the second biscuit is placed in a hot-pressing sintering furnace, the second biscuit is heated to 800 ℃ at the speed of 1 ℃/min and is kept warm for 6-8h, various organisms added are removed, so that the ceramic biscuit without residual carbon is obtained, then the ceramic biscuit without residual carbon is heated to 1600-1860 ℃ at the speed of 2-5 ℃/min, hot-pressing sintering is carried out in the heating process, the hot-pressing sintering time is 4-6 hours, then the temperature is reduced to 1600 ℃ at the speed of 2-4 ℃/min, and finally the ceramic biscuit is cooled to room temperature along with the furnace, so that the eutectic aluminum nitride ceramic heating structure device is obtained.
Preferably, in the technical scheme, after the step S09, the shape of the full aluminum nitride ceramic heating structure device is modified.
A full aluminum nitride ceramic heating structure device is prepared by the preparation method.
Compared with the prior art, in the preparation process of the scheme, the powder blank is densified by using heat energy, the longitudinal direction of the blank is reduced under the high-temperature condition, the porosity is reduced, the blank is densified, and the mechanical properties (mechanical strength and the like) are improved. The aluminum nitride green body and the conductive green body are subjected to a series of physical changes in the sintering process, such as expansion, contraction, gas generation, appearance of liquid phase, disappearance of old crystal phase, formation of new crystal phase, mutual interweaving and mutual infiltration of green bodies made of different materials on an interface and the like. Thereby forming eutectic ceramics with special crystalline phase composition and microstructure. The invention has the following beneficial effects:
the thermal and mechanical properties of the product are greatly improved, so that the product has the excellent characteristics of low heat capacity, low energy consumption, high thermal emissivity, high electrothermal efficiency, small thermal expansion coefficient, no deformation at high temperature, light weight, high power, energy conservation, no pollution, safety, reliability and the like, and can meet the technical requirements on heating structure devices in modern semiconductor manufacturing technological innovation.
Description of the drawings:
FIG. 1 is a metallographic structure diagram of a device with a full aluminum nitride ceramic heating structure according to the present invention.
FIG. 2 is an enlarged metallographic structure diagram of a device with a full aluminum nitride ceramic heating structure according to the present invention.
The specific implementation mode is as follows:
the following detailed description of specific embodiments of the invention is provided, but it should be understood that the scope of the invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
EXAMPLE 1 preparation of aluminum nitride insulating ceramic powder
S01: 95 percent of aluminum nitride powder (D50 =1.2-1.9 um) and 5 percent of Y 2 O 3 Ball milling the powder, butanone, absolute ethyl alcohol, polyvinyl butyral and castor oil for 15 hours by a ball mill to obtain mixed slurry;
s02: and carrying out spray granulation on the mixed slurry to obtain the aluminum nitride insulating ceramic powder.
Example 2 preparation of an aluminum nitride conductor material
S01: 75 percent of aluminum nitride powder (D50 =1.2-1.9 um) and 5 percent of Dy 2 O 3 Powder, 5% of Ti powder, 5% of Mo powder, 8% of Ta powder, 2% of Y 2 O 3 Ball milling the powder with butanone, absolute ethyl alcohol, polyvinyl butyral and castor oil for 25 hours by a ball mill to obtain mixed slurry;
s02: carrying out vacuum defoaming treatment on the mixed slurry to obtain a mixture, carrying out vacuum drying on the mixture, and carrying out spray granulation process to obtain aluminum nitride conductor powder with a certain sphericity;
s03: pressing and molding the aluminum nitride conductor powder to prepare a biscuit with a certain shape and size;
s04: placing the biscuit in a glue discharging furnace, and performing glue discharging treatment in a nitrogen atmosphere at 580 ℃ to discharge organic matters in the biscuit, thereby obtaining a ceramic biscuit without residual carbon;
s05: and placing the ceramic biscuit subjected to binder removal in a high-temperature graphite furnace, and sintering at 1850 ℃ for 6 hours in a nitrogen atmosphere to obtain the co-crystallized aluminum nitride conductor material.
Example 3 preparation of all-aluminum nitride ceramic heating Structure device
S01: pressing and molding aluminum nitride insulating ceramic powder to form a bottom layer, fixing an aluminum nitride conductor material in the bottom layer by pressing, coating the aluminum nitride insulating ceramic powder with the aluminum nitride conductor material to form a sandwich structure, and pressing and molding the sandwich structure to obtain a biscuit;
s02: placing the biscuit in a hot-pressing sintering furnace, carrying out binder removal in a nitrogen atmosphere, heating to 800 ℃ at the speed of 1 ℃/min, preserving heat for 6h, and removing various added organisms to obtain a ceramic biscuit without residual carbon;
s03: in the flow N 2 Under the protection of atmosphere, heating the ceramic biscuit to 1860 ℃ at the speed of 3 ℃/min, carrying out hot-pressing sintering in the heating process, wherein the hot-pressing sintering time is 6 hours, then cooling to 1600 ℃ at the speed of 3 ℃/min, and finally cooling to room temperature along with the furnace to obtain the all-aluminum nitride ceramic heating device, the metallographic structure of which is shown in figures 1 and 2, an aluminum nitride conductor can be seen from figure 1 to be wrapped by aluminum nitride insulating ceramic, and the upper aluminum nitride insulating ceramic and the lower aluminum nitride conductor interface can be seen from figure 2 to be mutually interwoven and mutually infiltrated.
In the preparation process of the full aluminum nitride ceramic heating structure device, the powder blank is densified by using heat energy, the longitudinal direction of the blank is reduced under the high-temperature condition, the porosity is reduced, the blank is densified, and the mechanical properties (mechanical strength and the like) are improved. A series of physical changes, such as expansion, contraction, gas generation, liquid phase appearance, disappearance of old crystal phase, formation of new crystal phase, mutual interweaving and mutual infiltration of blanks made of different materials at an interface, are generated in the sintering process of the aluminum nitride blank and the conductive blank. Therefore, the eutectic ceramic with special crystal phase composition and microstructure is formed, the thermal property and the mechanical property of the product are greatly improved, and the eutectic ceramic has the excellent characteristics of low heat capacity, low energy consumption, high thermal emissivity, high electrothermal efficiency, small thermal expansion coefficient, no deformation at high temperature, light weight, high power, energy conservation, no pollution, safety, reliability and the like, and can meet the technical requirements on heating structure devices in modern semiconductor manufacturing technological innovation.
The properties of the prepared full aluminum nitride ceramic heating device are shown in table 1:
TABLE 1
| Item | Performance of |
| Appearance of the product | Grey colour dense |
| Use voltage (V) | 110 |
| Resistance (omega) | 13 |
| Power of use (W) | 930 |
| Maximum service temperature (. Degree. C.) | 500 |
The foregoing description of specific exemplary embodiments of the invention has been presented for the purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (14)
1. A method for preparing a full aluminum nitride ceramic heating structure device comprises the following steps:
s01: mixing 94-99 wt% of aluminum nitride powder, 1-6 wt% of sintering aid, organic solvent, binder and dispersant by a ball mill to obtain first mixed slurry; the combustion improver is Y 2 O 3 、CaO、Li 2 O、YF 3 And CaF 2 Any one or a mixture of any several of them in any proportion;
s02: carrying out centrifugal atomization granulation on the first mixed slurry to obtain first powder with a certain sphericity;
s03: mixing 57-89 wt% of aluminum nitride powder, 10-40 wt% of metal powder, 1-3 wt% of sintering aid, organic solvent, binder and dispersant by a ball mill to obtain second mixed slurry; the metal powder is Ti, mo, ta, W, ni, co, dy 2 O 3 Any one or mixture of any several of them in any ratio; the combustion assistant agent is Y 2 O 3 、CaO、Li 2 O、YF 3 And CaF 2 Any one or a mixture of any several of them in any proportion;
s04: carrying out vacuum defoaming treatment on the second mixed slurry to obtain a mixture, carrying out post-treatment on the mixture, and carrying out crushing and granulation processes to obtain second powder with a certain sphericity;
s05: pressing and molding the second powder to prepare a first biscuit with a certain shape and size;
s06: placing the first biscuit in a glue discharging furnace for glue discharging treatment to discharge organic matters in the first biscuit, thereby obtaining a ceramic biscuit without residual carbon;
s07: placing the ceramic biscuit subjected to binder removal in a high-temperature furnace, and firing at high temperature in a nitrogen atmosphere to obtain a co-crystallized aluminum nitride-based conductive ceramic material;
s08: the first powder is pressed and formed to form a bottom layer, the aluminum nitride-based conductive ceramic material is fixed in the bottom layer through pressing, then the aluminum nitride-based conductive ceramic material is coated by the first powder to form a sandwich structure, and the sandwich structure is pressed and formed to obtain a second biscuit;
s09: and placing the second blank in a high-temperature furnace, and firing at high temperature in a nitrogen atmosphere to obtain the eutectic full aluminum nitride ceramic heating structure device.
2. The method of making a fully aluminum nitride ceramic heating structure device according to claim 1, wherein: the aluminum nitride powder is carbon reduction powder or powder generated by a direct nitridation method.
3. The method of making a fully aluminum nitride ceramic heating structure device according to claim 1, wherein: the organic solvent is butanone and/or absolute ethyl alcohol, the adhesive is polyvinyl butyral, and the dispersant is one or a mixture of any of fish oil, castor oil and triolein in any proportion.
4. The method of making a fully aluminum nitride ceramic heating structure device according to claim 1, wherein: in the step S01, the mixture is mixed into uniform slurry with certain viscosity and good fluidity on a ball mill in a wet ball milling mode, and the wet ball milling time is generally 5-20h.
5. The method of making a fully aluminum nitride ceramic heating structure device according to claim 1, wherein: and S02, putting the first mixed slurry into a spray granulation tower, and carrying out centrifugal atomization granulation at the inlet temperature of the spray granulation tower of 150-200 ℃ to form powder balls with a certain sphericity.
6. The method of making a fully aluminum nitride ceramic heating structure device according to claim 1, wherein: in step S03, the slurry is mixed into uniform slurry with certain viscosity and good fluidity by a wet ball milling method on a ball mill, wherein the wet ball milling time is generally 10-30h.
7. The method of making a fully aluminum nitride ceramic heating structure device according to claim 1, wherein: and S04, putting the mixture subjected to vacuum defoaming treatment into a high vacuum drying device for drying treatment, wherein the temperature of a heater is set to be less than or equal to 150 ℃, and the vacuum degree is set to be less than or equal to 0.01Mpa.
8. The method of making a fully aluminum nitride ceramic heating structure device according to claim 1, wherein: and S04, sieving the crushed and granulated powder to prepare second powder with a certain sphericity, wherein the particle size of the second powder is 60-200 meshes.
9. The method of making a fully aluminum nitride ceramic heating structure device according to claim 1, wherein: in step S06, the glue discharging treatment is carried out in nitrogen atmosphere at the temperature of less than or equal to 800 ℃.
10. The method of making a fully aluminum nitride ceramic heating structure device according to claim 1, wherein: and step S07, according to different ceramic formulas, performing high-temperature sintering in a graphite sintering furnace or a metal vacuum sintering furnace at 1600-1860 ℃ in a nitrogen atmosphere for 4-6 hours to obtain the eutectic aluminum nitride-based conductive ceramic material.
11. The method of making a fully aluminum nitride ceramic heating structure device according to claim 1, wherein: and step S08, processing the corresponding pattern on the aluminum nitride-based conductive ceramic material, carrying out rough grinding, cutting and slicing on the aluminum nitride-based conductive ceramic material, processing the conductive pattern, testing the resistance of the aluminum nitride-based conductive ceramic material in a partition mode according to the designed resistance, and then carrying out micro-polishing according to the actual resistance, so as to ensure that the resistance of the conductive pattern in all areas is consistent.
12. The method of making a fully aluminum nitride ceramic heating structure device according to claim 1, wherein: and step S09, placing the second biscuit in a hot-pressing sintering furnace, firstly heating to 800 ℃ at the speed of 1 ℃/min, preserving heat for 6-8h, removing various organisms added, thus obtaining the ceramic biscuit without residual carbon, then heating to 1600-1860 ℃ at the speed of 2-5 ℃/min, carrying out hot-pressing sintering in the heating process, wherein the hot-pressing sintering time is 4-6 hours, then cooling to 1600 ℃ at the speed of 2-4 ℃/min, and finally cooling to room temperature along with the furnace, thus obtaining the eutectic aluminum nitride ceramic heating structure device.
13. The method of making a fully aluminum nitride ceramic heating structure device according to claim 1, wherein: and step S09, performing appearance modification on the full aluminum nitride ceramic heating structure device.
14. The utility model provides a full aluminium nitride ceramic heating structure device which characterized in that: prepared by the preparation method of any one of claims 1 to 13.
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| CN112573926A (en) * | 2020-12-28 | 2021-03-30 | 无锡海古德新技术有限公司 | Aluminum nitride conductor material and aluminum nitride full-ceramic heating structure device |
| CN112811910A (en) * | 2021-03-26 | 2021-05-18 | 无锡海古德新技术有限公司 | Aluminum nitride-based functional ceramic material and preparation method thereof |
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| US6133557A (en) * | 1995-01-31 | 2000-10-17 | Kyocera Corporation | Wafer holding member |
| CN101333114A (en) * | 2008-07-31 | 2008-12-31 | 潮州三环（集团）股份有限公司 | Method for making high-thermal-conductivity aluminium nitride ceramics substrate |
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