CN106986665B - Preparation method of 99.6% Al2O3 ceramic substrate for thin film integrated circuit - Google Patents
Preparation method of 99.6% Al2O3 ceramic substrate for thin film integrated circuit Download PDFInfo
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- CN106986665B CN106986665B CN201710305151.1A CN201710305151A CN106986665B CN 106986665 B CN106986665 B CN 106986665B CN 201710305151 A CN201710305151 A CN 201710305151A CN 106986665 B CN106986665 B CN 106986665B
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- 239000000758 substrate Substances 0.000 title claims abstract description 101
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000000919 ceramic Substances 0.000 title claims abstract description 50
- 239000010409 thin film Substances 0.000 title claims abstract description 34
- 229910052593 corundum Inorganic materials 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 229910001845 yogo sapphire Inorganic materials 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 38
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- 239000002002 slurry Substances 0.000 claims description 21
- 238000005498 polishing Methods 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- 238000004528 spin coating Methods 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 15
- 239000003960 organic solvent Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000005266 casting Methods 0.000 claims description 11
- 229910052681 coesite Inorganic materials 0.000 claims description 11
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- 238000002156 mixing Methods 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 238000005245 sintering Methods 0.000 claims description 11
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- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 7
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- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
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- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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- H01L21/70—Manufacture or treatment of devices consisting of a plurality of solid state components formed in or on a common substrate or of parts thereof; Manufacture of integrated circuit devices or of parts thereof
- H01L21/77—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate
- H01L21/78—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate with subsequent division of the substrate into plural individual devices
- H01L21/82—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate with subsequent division of the substrate into plural individual devices to produce devices, e.g. integrated circuits, each consisting of a plurality of components
- H01L21/84—Manufacture or treatment of devices consisting of a plurality of solid state components or integrated circuits formed in, or on, a common substrate with subsequent division of the substrate into plural individual devices to produce devices, e.g. integrated circuits, each consisting of a plurality of components the substrate being other than a semiconductor body, e.g. being an insulating body
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Abstract
The invention provides 99.6% Al for thin film integrated circuit2O3A method for preparing a ceramic substrate. The thin film integrated circuit provided by the invention uses 99.6% Al2O3The preparation method of the ceramic substrate can reduce the surface roughness of the substrate and improve the smoothness and the flatness, thereby improving the precision and the reliability of the thin film circuit and having important practical value. Meanwhile, the thin film integrated circuit provided by the invention is 99.6% of Al2O3The preparation method of the ceramic substrate has the advantages of small surface roughness, good flatness, good finish, mirror surface on the surface and the like.
Description
Technical Field
The invention relates to the field of microwave medium ceramic substrates for thin film hybrid integrated circuits, in particular to 99.6 percent Al for a thin film integrated circuit2O3A method for preparing a ceramic substrate.
Background
99.6%Al2O3The electronic ceramic substrate has the advantages of high temperature resistance, high electrical insulation performance, low dielectric loss, large thermal conductivity, strong chemical stability, thermal expansion coefficient similar to that of elements and the like, thereby being widely applied to thick/thin film hybrid integrated circuits and various thin film components.
However, because the 99.6% alumina ceramic substrate has high hardness and large crystal grains, the surface smoothness of the substrate after processing is difficult to achieve the mirror effect (< 0.02 μm), and even if the ceramic substrate is mechanically thinned and polished, micron-sized holes still exist on the surface, so that holes, defects, electrode loss, disconnection or short circuit easily occur in a thin film circuit, and the reliability of the thin film circuit is seriously influenced. With the rapid development of microwave components and devices, the micro-machining technology is changing day by day, and the design of thin film components requires that an alumina ceramic substrate has better finish and very small surface roughness, so that the nano-scale circuit line width is met. The alumina substrate after mechanical thinning and polishing can meet the requirements of common circuit design, but the line width can not meet the requirements of nano-scale thin film circuits. Therefore, the surface of the thinned alumina ceramic substrate needs to be further subjected to finish machining, so that the surface roughness is reduced and the mirror surface effect is achieved.
At present, the surface roughness of an alumina ceramic substrate can not meet the design requirement of a thin film circuit, almost all the performances can meet the design requirement, and in order to solve the problem, the traditional chemical mechanical polishing method is mainly adopted. Although the chemical mechanical polishing can reduce the roughness of the surface of the substrate, the roughness after polishing can only reach 0.04-0.05 mu m due to the higher hardness of the alumina substrate, the mirror surface effect is not obvious, the consumed polishing solution is more, the cost is high, the polishing time is long, the efficiency is low, and the experimental statistics shows that 1 piece of 99.6 percent Al is polished2O3The time of the ceramic substrate exceeds 2 h. Meanwhile, although the prior art also has a method for depositing a layer of film on the surface of the substrate by using a special technical means, the prior art requires expensive equipment, complex technology and high cost, and is not suitable for practical production application.
Therefore, the surface treatment process and performance index of the existing alumina ceramic substrate are difficult to meet the application requirements of high-performance thin film devices/circuits, and a new process is urgently needed to be found to improve the surface roughness and the smoothness of the thin film devices/circuits so as to meet the requirements of the thin film devices/circuits on the substrates with high reliability, low cost and high appearance quality.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the present invention is to provide 99.6% Al for a thin film integrated circuit2O3Method for preparing ceramic substrates by applying 99.6% Al2O3The surface of the ceramic substrate is subjected to mirror surface treatment, so that the surface roughness of the ceramic substrate can be reduced, and the smoothness of the substrate can be improved.
The second purpose of the invention is to provide 99.6% Al for the thin film integrated circuit2O3The ceramic substrate provided by the invention has the advantages of small surface roughness, high smoothness and the like, and is suitable for precise electronic components such as a nano-scale thin film circuit and the like.
It is a third object of the present invention to provide a semiconductor device comprising 99.6% Al for the thin film integrated circuit2O3An electronic component with a ceramic substrate.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
99.6% Al for thin film integrated circuit2O3A method for preparing a ceramic substrate, said method comprising the steps of:
(a)99.6%Al2O3ceramic substrate preparation
According to Al2O3MgO and SiO2Proportioning 99.6 wt% to 0.3 wt% to 0.1 wt%, ball milling the mixture with agate balls and deionized water, drying and sieving;
mixing the dried and sieved material with an organic solvent and an adhesive to prepare a casting material, then carrying out casting molding to obtain an alumina green tape, and carrying out lamination, isostatic pressing, cutting and binder removal sintering on the obtained alumina green tape to obtain 99.6% Al2O3Thinning and polishing the ceramic substrate, and ultrasonically washing to obtain an alumina ceramic substrate to be treated;
(b) preparation of high-softening degree glass powder
CaO 10-30 wt%, and Al2O30~18.3%,SiO254.93-74.93%, and glass additive 10 c25 percent of the raw materials are mixed, the obtained materials are subjected to high-temperature water quenching to obtain a glass body, the obtained glass body is vibrated, ground and added with a dispersion medium for ball milling, and then dried and sieved to obtain glass powder;
(c) glass paste preparation
Dissolving an organic carrier in a solvent, adding glass powder into the obtained solution, and uniformly dispersing to obtain glass slurry;
(d) glue homogenizing
Spin-coating glass slurry on the surface of an alumina ceramic substrate to be treated, and then drying the obtained substrate;
(e) thermal treatment
Placing the dried substrate in a muffle furnace for heat treatment to obtain an alumina ceramic substrate with high surface smoothness, namely 99.6 percent Al for the thin film integrated circuit2O3A ceramic substrate.
Optionally, in the invention, in the step (a), the mass ratio of the material, the agate balls and the deionized water is (1-2) to (1-2);
and/or the ball milling rotation speed of the ball milling mixing in the step (a) is 350-450 rpm, and the time is 5-6 h.
Optionally, in the present invention, the thinning and polishing in the step (a) is to obtain 99.6% Al2O3Thinning and polishing the two sides of the ceramic substrate;
preferably, the thickness of the alumina ceramic substrate to be treated is less than 1mm after thinning, polishing and ultrasonic washing, and the thickness precision and uniformity are less than +/-3 μm.
Optionally, in the present invention, the glass additive in step (b) is BaO, MgO, ZnO, Sb2O3Or B2O3One or a mixture of several of them.
Optionally, in the present invention, the dispersion medium in step (b) is an organic solvent, and preferably, the dispersion medium is an ethanol solution;
and/or the rotation speed of the ball milling in the step (b) is 350-450 rpm, and the time is 2-4 h.
Optionally, in the present invention, all the organic carriers in step (c) are ethyl cellulose, acrylic resin, or polyvinyl butyral;
the solvent is a mixed solvent of terpineol and butyl carbitol;
preferably, the mass ratio of the terpineol, the butyl carbitol and the organic carrier is (35-48): (33-49): 4-15).
Optionally, in the present invention, in the step (d), the glass slurry is spin-coated by using a spin coating method;
preferably, the spin-coating speed is 500-1500 rpm, the time is 10-20 s, and the times are 1-6.
Optionally, in the present invention, the heat treatment in step (e) specifically includes the following steps: heating a muffle furnace from room temperature to 500-600 ℃, and controlling the heating time to be 6-8 h; then heating to 900-1000 ℃, and controlling the heating time to be 2-3 h; then heating to 1150-1300 ℃, and controlling the heating time to 80-90 min; and keeping the temperature for 30-45 min and then cooling along with the furnace.
The invention also provides 99.6 percent Al for the thin film integrated circuit prepared by the method2O3A ceramic substrate.
Further, the invention also provides 99.6 percent of Al for the thin film integrated circuit2O3An electronic component with a ceramic substrate.
Compared with the prior art, the invention has the beneficial effects that:
in the invention, the ceramic sintered alumina ceramic is thinned, the parts of the surface of the substrate which are not compact in sintering and uneven in sintering are removed, and a uniform glass glaze layer is formed on the surface of the substrate in glue homogenizing and heat treatment modes, so that the surface smoothness of the substrate is further improved;
meanwhile, the CaO-Al adopted by the invention2O3-SiO2The glass has high softening point, thermal expansion coefficient and Al2O3The method has the characteristics of being close to the prior art, and compared with the traditional screen printing method, the method of coating by adopting the glue homogenizing method has the advantages of smooth surface, extremely thin and uniform thickness and the like; can obtain super-smooth surface after heat treatmentThe alumina ceramic also has important practical value for the design, assembly and further application of precise electronic components such as thin film integrated circuits and the like
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 shows 99.6% Al of an uncoated glass glaze2O3A ceramic substrate;
FIG. 2 shows 99.6% Al of a spin-on glass glaze2O3A ceramic substrate.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In view of the shortcomings of the existing alumina ceramic substrate in performance and preparation process, related researchers in the field of alumina ceramic substrates have conducted intensive research on the aspect of substrate surface treatment, common methods include polishing methods and surface coating methods, the coating technologies mainly include Chemical Vapor Deposition (CVD), Physical Vapor Deposition (PVD), thermal spraying methods, screen printing methods, sol-gel methods and the like, and with the development of modern ceramic glaze technology, the glass glaze technology has been applied to the fields of insulating layer preparation and electronic device packaging. The glass glaze is a thin and uniform glass substance fused on the surface of the substrate, and has the characteristics of smoothness, brightness, high mechanical strength, stable chemical property, good matching with the substrate and the like, but the reports of coating high-temperature glass glaze on the surface of the alumina ceramic substrate at home and abroad are few at present, and the invention provides 99.6 percent Al with small surface roughness and high smoothness through related research and test under the background2O3Ceramic substrate preparation methodSpecifically, the method of the invention comprises the following steps:
1、99.6%Al2O3ceramic substrate preparation
1.1 according to Al2O3MgO and SiO2Proportioning 99.6 percent by mass, 0.3 percent by mass and 0.1 percent by mass, and then ball-milling and mixing the obtained material with agate balls and deionized water;
preferably, the mass ratio of the materials to the agate balls to the deionized water is (1-2) to (1-2); more preferably, the mass ratio of the materials, the agate balls and the deionized water is 1:2: 1;
preferably, in the step, the raw materials are weighed according to the proportion and then are subjected to ball milling and mixing in an agate tank;
preferably, the ball milling rotation speed of the ball milling mixing is 350-450 rpm, and the time is 5-6 h; more preferably, the ball milling rotation speed of the ball milling mixing is 387rpm, and the time is 6 h;
after ball milling, pouring out the obtained slurry, drying and sieving;
preferably, the drying is drying, the obtained slurry is dried for 48 hours at the constant temperature of 90 ℃, and then the slurry passes through a 100-mesh screen;
1.2, mixing the dried and sieved material with an organic solvent and an adhesive to prepare a casting material, wherein the preparation of the casting material can refer to the preparation process of a conventional casting material, the used organic solvent can be organic solvents such as toluene, ethanol and the like, and the used adhesive can be an adhesive such as PVB and the like;
preparing an alumina raw porcelain band from the casting material through a tape casting forming method, processing the obtained alumina raw porcelain band through the procedures of lamination, isostatic pressing and cutting to obtain a square alumina block, and placing the formed alumina block in a high-temperature sintering furnace for binder removal sintering to obtain the alumina green porcelain band with the content of 99.6 percent Al2O3A ceramic substrate;
preferably, the glue discharging temperature is 600 ℃, the heat preservation is carried out for 4 hours, the sintering temperature is 1580 ℃, and the heat preservation is carried out for 2 hours;
then, the obtained 99.6% Al was added2O3The ceramic substrate is thinned and polished to remove the sintering incompact and uneven parts on the surface of the sample;
preferably, the thinning and polishing are performed on the obtained 99.6% Al2O3Thinning and polishing the two sides of the ceramic substrate;
after thinning and polishing, carrying out ultrasonic cleaning on the ceramic substrate to obtain an alumina ceramic substrate to be treated, wherein the thickness of the obtained substrate is less than 1mm, the thickness precision and uniformity are less than +/-3 microns, and the roughness is less than 0.1 micron;
preferably, the cleaning time is controlled to be about 30 min;
2. preparation of high-softening degree glass powder
Due to CaO-Al2O3-SiO2The glass has a high melting point (over 1100 ℃), and is mixed with 99.6% Al2O3The thermal expansion coefficient of the ceramic is close to that of the ceramic, and the thermal expansion coefficient is 6-8 multiplied by 10-6In the range of/° c; therefore, CaO-Al is selected by the invention2O3-SiO2Is a glass glaze, and is prepared from (by mass) CaO 10-30%, and Al according to ternary phase diagram2O30~18.3%,SiO254.93-74.93% and 10-25% of glass additive; the glass formula can be further adjusted to change the softening point of the glass, so that the glass is suitable for heat treatment at different temperatures;
preferably, the glass additive is BaO, MgO, ZnO, Sb2O3Or B2O3One or a mixture of several of them;
placing the weighed materials in a ball milling tank, and carrying out ball milling and mixing; then the ingredients after ball milling are put into a corundum crucible of a frit furnace, and are melted in a high-temperature frit furnace to generate glass, and the glass is poured into deionized water for quenching treatment after the melting is finished to obtain a colorless and transparent glass body, namely, the glass body is prepared by adopting a high-temperature water quenching (high-temperature melting water quenching) method; the obtained glass body is vibrated, ground and crushed, then a dispersion medium is added for ball milling, and the glass powder is obtained after drying and sieving;
preferably, the dispersion medium is an organic solvent, and preferably, the dispersion medium is an ethanol solution;
preferably, the rotation speed of the ball mill is 350-450 rpm, the time is 2-4 h, and the aperture of a screen used for sieving is 300 meshes; more preferably, the rotation speed of the ball mill is 387rpm, the time is 2-4 h, and the glass powder is obtained by screening through a dried 300-mesh stainless steel screen;
3. glass paste preparation
In the step, firstly, an organic carrier solution is prepared, preferably, the organic carrier is added into a solvent loaded in a beaker, and then the mixture is stirred for 1 to 3 hours to be dissolved under the condition of heating in a water bath at the temperature of 50 to 80 ℃;
preferably, the organic solvent used is terpineol and butyl carbitol; preferably, the organic carrier used is ethyl cellulose, acrylic resin, or polyvinyl butyral;
further preferably, the mass ratio of the terpineol, the butyl carbitol and the organic carrier (namely ethyl cellulose, acrylic resin or polyvinyl butyral) is (35-45): (33-44): (4-15);
then, the glass powder prepared in the step 2 is placed in a beaker according to the proportion of 40-60 percent of solid content to be stirred and dispersed uniformly to prepare glass slurry, and the prepared glass slurry has good suspension property and uniform dispersion and is suitable for spin coating on an alumina ceramic substrate;
4. glue homogenizing
Spin-coating glass slurry on the surface of an alumina ceramic substrate to be treated, preferably, in the step, spin-coating the glass slurry by a glue-homogenizing method, and enabling the surface of the substrate to be smooth and uniform;
preferably, the glue homogenizing speed is 500-1500 rpm, the time is 10-20 s, the frequency is 1-6, and the frequency of glue homogenizing can be controlled according to needs;
then drying the obtained substrate, preferably, the drying is to bake the substrate on a hot plate for 3min, and the temperature of the hot plate is controlled to be 130-200 ℃;
5. thermal treatment
Placing the dried substrate in a muffle furnace for heat treatment, wherein after the heat treatment, a layer of glass glaze is formed on the surface of the substrate by the spin-coated glass slurry, the smoothness is high, the surface roughness is less than 0.01 mu m, and the thickness precision of the substrate is less than +/-2 mu mm is 99.6% Al for thin film integrated circuit2O3A ceramic substrate;
preferably, the heat treatment comprises the steps of: heating a muffle furnace from room temperature to 500-600 ℃, and controlling the heating time to be 6-8 h; then heating to 900-1000 ℃, and controlling the heating time to be 2-3 h; then heating to 1150-1300 ℃, and controlling the heating time to 80-90 min; keeping the temperature for 30-45 min and then cooling along with the furnace;
more preferably, the heat treatment temperature increasing step is as follows: firstly, heating the muffle furnace from room temperature to 600 ℃, and controlling the heating time to be 8 h; then heating to 1000 ℃, and controlling the heating time to be 2 h; then heating to 1150-1300 ℃, and controlling the heating time to 80 min; keeping the temperature for 30min and then cooling the mixture along with the furnace.
Al prepared by the above method2O3The ceramic substrate has small surface roughness and high substrate thickness precision, so that the ceramic substrate is suitable for serving as a nano-scale thin film circuit substrate, and the precision and the reliability of a thin film circuit are improved. Also, the resin composition is used as a base material or a packaging material for other precision electronic components.
Example 1
(1) Proportioning and mixing materials
Raw materials are according to 99.6 percent of Al2O3-0.3%MgO-0.1%SiO2The materials are mixed according to the mass ratio, and the weighed mixture, the agate balls and the deionized water are put into an agate tank according to the ratio of 1:2:1 for ball milling and mixing;
the ball milling parameters are as follows: 387rpm for 6 hours, pouring out the slurry after ball milling, putting the slurry into an oven, drying the slurry for 48 hours at the constant temperature of 90 ℃, and sieving the dried slurry by a 100-mesh sieve;
(2) preparation of casting material
Adding organic solvents ethanol and toluene and an adhesive PVB into the alumina powder obtained after drying and sieving to obtain a casting material;
(3) casting and laminating
Adopting a tape casting forming method, preparing an alumina green porcelain tape by a tape casting machine from a tape casting material, wherein the film thickness is 59 +/-1 mu m, then laminating 9 layers, and then carrying out isostatic pressing and cutting processes to obtain a square alumina block, wherein the thickness is 445 mu m, and the size is 61 multiplied by 61 mm;
(4) binder removal and sintering
And (3) placing the formed alumina bar block into a muffle furnace for air atmosphere sintering, wherein the temperature rise curve is as follows: the room temperature is increased to 600 ℃ within 10h, the temperature is kept for 4h, the temperature is increased to 1300 ℃ within 3h, the temperature is increased to 1580 ℃ within 2h, the temperature is kept for 2h, the temperature is reduced to 1000 ℃ within 2h, and the ceramic is cooled along with the furnace to obtain 99.6 percent Al sintered into ceramic2O3A ceramic substrate having a thickness of 350 μm and dimensions of 50.8 × 50.8 mm;
(5) thinning
Thinning and polishing the two sides of the sintered ceramic alumina substrate by using a thinning machine, removing the sintering incompact and uneven parts on the surface, and then ultrasonically cleaning for 30min to obtain the ceramic substrate with the thickness of 300 mu m, the thickness precision and uniformity of less than +/-3 mu m and the surface roughness of less than 0.1 mu m, wherein the obtained substrate is shown in figure 1;
(7) preparation of high-temperature glass powder
Preparing raw materials of each component of glass according to the mass fraction ratio in the table 1; then placing the mixture into a ball milling tank, carrying out ball milling for 6 hours to uniformly mix all the components, and screening the mixture through a 40-mesh screen after ball milling and drying;
TABLE 1 glass formulation
Then, the ingredients after ball milling are put into a corundum crucible of a frit furnace and are melted in a high-temperature frit furnace to generate glass, the melting temperature is 1450 ℃, and the heat preservation time is 1 h; pouring the molten glass into deionized water for quenching treatment after the melting is finished to obtain colorless and transparent glass bodies, then performing vibromilling and crushing, performing ball milling for 2-4 h at 387rpm by using alcohol as a dispersion medium, and drying and then sieving the glass bodies by using a 300-mesh stainless steel sieve to obtain glass powder;
(8) preparation of glass paste
Weighing an organic solvent and ethyl cellulose according to the proportion in the following table 2, placing the organic solvent and the ethyl cellulose in a beaker, stirring the mixture in a water bath at the temperature of 80 ℃ for 2 hours until the mixture is completely dissolved, and then placing glass powder in the beaker according to the proportion of 40-60% of solid content, and uniformly stirring and dispersing the glass powder to obtain glass slurry;
TABLE 2 organic vehicle ratios
Organic solvent | Terpineol | Butyl carbopipanol | Ethyl cellulose |
W% | 44 | 46 | 10 |
(9) Glue homogenizing
Uniformly spin-coating the prepared glass slurry on the surface of the alumina ceramic substrate prepared in the step (5) by using a spin coater, wherein the spin coating speed is 1000rpm, the spin coating time is 20s, the spin coating frequency is 1 time, and after the spin coating is finished, the substrate is placed on a hot plate and baked for 3min for later use;
(10) thermal treatment
Placing the substrate after glue homogenizing in a muffle furnace for heat treatment, wherein the heat treatment curve is as follows: the room temperature is 8h to 600 ℃, then 2h is increased to 1000 ℃, the temperature is increased to 1200 ℃ in 80min, the temperature is kept for 30min, and then the film integrated circuit is cooled along with the furnace, thus obtaining the 99.6 percent Al for the film integrated circuit2O3A ceramic substrate;
the thickness of the obtained substrate is 303 micrometers, namely, the thickness of the glass glaze layer which is uniformly glued for 1 time is 3 micrometers after heat treatment, the thickness precision is +/-2 micrometers, and the surface roughness is 0.008 micrometers;
the obtained substrate has good surface finish, and its surface structure is shown in FIG. 2, wherein the white part is the reflected light after the substrate surface reaches mirror effect.
Example 2
Changing the composition of the glass: according to the basic formula, in CaO-Al2O3-SiO2The composition and the content of the additives in the glass phase forming interval are changed as shown in the following table:
table 3 modified glass formulation design
Then the ingredients are put into a corundum crucible of a frit furnace and melted in a high-temperature frit furnace to generate glass, the melting temperature is changed to 1500 ℃, and the heat preservation time is 1 h. After the melting is finished, pouring the mixture into deionized water for quenching treatment to obtain a colorless and transparent glass body. The glass slurry is prepared after ball milling, then the glass slurry is uniformly coated on the surface of the substrate by spin coating through spin coating, and then the heat treatment is carried out, wherein the heat treatment temperature is changed to 1250 ℃, other process conditions are not changed, and the specific operation process is the same as that of the embodiment 1.
The surface of the substrate after heat treatment has high smoothness and mirror effect, the surface roughness is 0.007 mu m, the thickness of the substrate is 303 mu m, and the thickness precision is +/-2 mu m.
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (13)
1. 99.6% Al for thin film integrated circuit2O3Method for the preparation of a ceramic substrate, characterized in that it comprises the following steps:
(a)99.6%Al2O3ceramic substrate preparation
According to Al2O3MgO and SiO2Proportioning 99.6 wt% to 0.3 wt% to 0.1 wt%, ball milling the mixture with agate balls and deionized water, drying and sieving;
drying and sievingMixing the material with organic solvent and adhesive to prepare casting material, then carrying out casting molding to obtain alumina green porcelain tape, and carrying out lamination, isostatic pressing, cutting and binder removal sintering on the obtained alumina green porcelain tape to obtain 99.6% Al2O3Thinning and polishing the ceramic substrate, and ultrasonically washing to obtain an alumina ceramic substrate to be treated;
(b) preparation of high-softening degree glass powder
CaO 10-30 wt%, and Al2O30~18.3%,SiO254.93-74.93% and 10-25% of glass additive, performing high-temperature water quenching on the obtained material to obtain a glass body, performing vibration milling and crushing on the obtained glass body, adding a dispersion medium, performing ball milling, drying and sieving to obtain glass powder;
(c) glass paste preparation
Dissolving an organic carrier in a solvent, adding glass powder into the obtained solution, and uniformly dispersing to obtain glass slurry;
(d) glue homogenizing
Spin-coating glass slurry on the surface of an alumina ceramic substrate to be treated, and then drying the obtained substrate;
(e) thermal treatment
Placing the dried substrate in a muffle furnace for heat treatment to obtain an alumina ceramic substrate with high surface smoothness, namely 99.6 percent Al for the thin film integrated circuit2O3A ceramic substrate.
2. The preparation method of claim 1, wherein in the step (a), the mass ratio of the material to the agate balls to the deionized water is (1-2): 1-2;
and/or the ball milling rotation speed of the ball milling mixing in the step (a) is 350-450 rpm, and the time is 5-6 h.
3. The method of claim 1, wherein the thinning polishing in step (a) is performed to obtain 99.6% Al2O3And thinning and polishing the two sides of the ceramic substrate.
4. The method for preparing the alumina ceramic substrate according to claim 3, wherein the thickness of the alumina ceramic substrate to be treated is less than 1mm after thinning, polishing and ultrasonic washing, and the thickness precision and uniformity are less than +/-3 μm.
5. The method according to claim 1, wherein the glass additive in step (b) is BaO, MgO, ZnO, Sb2O3Or B2O3One or a mixture of several of them.
6. The production method according to claim 5, wherein the dispersion medium in the step (b) is an organic solvent; and/or the rotation speed of the ball milling in the step (b) is 350-450 rpm, and the time is 2-4 h.
7. The method according to claim 6, wherein the dispersion medium in the step (b) is an ethanol solution.
8. The method according to claim 1, wherein the organic vehicle in the step (c) is ethyl cellulose, an acrylic resin, or polyvinyl butyral;
the solvent is a mixed solvent of terpineol and butyl carbitol.
9. The method according to claim 8, wherein the mass ratio of terpineol, butyl carbitol and organic carrier is (35-48): (33-49): (4-15).
10. The method according to claim 1, wherein the spin coating speed is 500 to 1500rpm, the time is 10 to 20s, and the number of spin coating times is 1 to 6.
11. The method according to claim 1, wherein the heat treatment in the step (e) specifically comprises the steps of: heating a muffle furnace from room temperature to 500-600 ℃, and controlling the heating time to be 6-8 h; then heating to 900-1000 ℃, and controlling the heating time to be 2-3 h; then heating to 1150-1300 ℃, and controlling the heating time to 80-90 min; and keeping the temperature for 30-45 min and then cooling along with the furnace.
12. 99.6% Al for thin film integrated circuits produced by the method according to any one of claims 1 to 112O3A ceramic substrate.
13. 99.6% Al for a thin film integrated circuit according to claim 122O3An electronic component with a ceramic substrate.
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CN1911859A (en) * | 2005-08-09 | 2007-02-14 | 黄荣厦 | Curtain casting preparation method of ceramic film sheet for electronic device |
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