CN114800775B - GSPL-SNST silicon nitride tape casting biscuit and preparation method thereof - Google Patents
GSPL-SNST silicon nitride tape casting biscuit and preparation method thereof Download PDFInfo
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- CN114800775B CN114800775B CN202210563003.0A CN202210563003A CN114800775B CN 114800775 B CN114800775 B CN 114800775B CN 202210563003 A CN202210563003 A CN 202210563003A CN 114800775 B CN114800775 B CN 114800775B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B1/00—Producing shaped prefabricated articles from the material
- B28B1/29—Producing shaped prefabricated articles from the material by profiling or strickling the material in open moulds or on moulding surfaces
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B3/00—Producing shaped articles from the material by using presses; Presses specially adapted therefor
- B28B3/003—Pressing by means acting upon the material via flexible mould wall parts, e.g. by means of inflatable cores, isostatic presses
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
- C04B35/587—Fine ceramics
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Abstract
The invention provides a preparation method of a GSPL-SNST silicon nitride tape casting biscuit, which comprises the following steps: GSPL-SNCS slurry prepared by SDPR pretreatment system and/or HVCM pretreatment system and/or GSPL production line is defoamed in vacuum, casted and dried to form the slurry with the thickness ofT 0 The first biscuit of (a). And cutting and neatly stacking the N layers of the first biscuit after the film belts are removed, sealing the first biscuit by using a PET vacuum packaging bag, and placing the first biscuit in an isostatic press for static pressure for 5 to 40 minutes under the pressure of 1 to 40MPa to form a second biscuit formed by fusing a plurality of layers of the first biscuit. The first embryo produced by the method has better performance in all aspects than the previous embryo, and multiple layers of embryos are fused by an isostatic press, so that the properties of each embryo are almost completely consistent during slicing, the roughness is small, and obvious layering and air hole phenomena are avoided. The required thickness can be customized according to the needs, and no waste is generated.
Description
Technical Field
The invention relates to the technical field of silicon nitride slurry casting, in particular to a GSPL-SNST silicon nitride casting biscuit and a preparation method thereof.
Background
With the miniaturization of electronic components and the rapid development of large-scale integrated circuits, higher demands are being made on ceramic substrates as important pillars of integrated circuits. In some special fields, the ceramic substrate is required to have not only good heat conductivity but also higher strength. The ceramic substrate material widely used at present is mainly A1 2 O 3 However, al 2 O 3 The substrate has the disadvantages of low thermal conductivity, large dielectric constant, large difference between the linear expansion coefficient and the linear expansion coefficient of the silicon element, and the like, and other materials replacing the alumina substrate are developed and researched in recent years, wherein the silicon nitride ceramic substrate not only has high thermal conductivity, but also has higher strength. The core technology of ceramic substrate preparation is the molding of a high-quality substrate blank, the current molding method mainly comprises tape casting, dry pressing and film rolling, and the tape casting method has high production efficiency, is easy to realize continuous production and automation, is more suitable for industrial large-scale production, and is an ideal ceramic substrate production technology. In the casting production process, a casting biscuit needs to be manufactured firstly, the casting biscuit is sintered to manufacture the silicon nitride ceramic substrate, and the quality of the manufactured casting biscuit directly influences various performances of the generated ceramic substrate.
The prior casting biscuit has the following problems in the preparation process: firstly, when the thickness of a substrate customized by a customer is thick, a casting biscuit produced in the prior art is often a biscuit with the thickness of the customized substrate which cannot be generated by casting at one time, and a plurality of biscuits are often required to be fused into a biscuit meeting the specification, but the roughness of the biscuit generated in the prior art is large, and the layering phenomenon and the air hole phenomenon occur inside the biscuit; secondly, the thickness of the casting biscuit generated in the prior art is often adjusted and controlled through the adjusting coefficient of the casting equipment, the adjusting coefficient is directly calculated according to the generated slurry in the prior art, the casting thickness is controlled to meet the requirements, in order to achieve the casting biscuit meeting the customized thickness, different adjusting coefficients are repeatedly adjusted by using a pre-experiment in the prior art to adjust the thickness, the adjusting coefficient meeting the requirements is determined, repeated experiments often cause the waste of the casting biscuit, the consumed time is long, and the workload is large.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a GSPL-SNST silicon nitride casting biscuit and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme: the preparation method of the GSPL-SNST silicon nitride casting biscuit comprises the following steps:
s1: preparation of a first biscuit:
treating inorganic solid raw material with SDPR pretreatment system, treating organic additive with HVCM pretreatment system to generate organic colloid, mixing the organic colloid and the inorganic solid raw material with GSPL production line to obtain GSPL-SNCS slurry, vacuum defoaming, casting and drying to obtain GSPL-SNCS slurry with thickness ofT 0 A first biscuit of (a);
the SDPR pretreatment system, the HVCM pretreatment system and the GSPL production line equipment are designed and produced by ecological environment science and technology limited corporation of Jiangsu Fangzheng tableland.
The inorganic solid at least comprises Si 3 N 4 Powder and inorganic sintering aid powder;
the organic colloid at least comprises a mixture of castor oil, absolute ethyl alcohol, polymethyl propylene, polyethylene glycol and glycerol monooleate;
before production, the inorganic solid and the organic additive are respectively pretreated by equipment and then mixed, so that the problems that in the prior art, various raw materials are directly mixed to prepare slurry, and the performance of the first blank generated by the production flow of the slurry prepared by an equipment production line is superior to that of the previous blank in all aspects are solved.
S2: preparation of a second biscuit:
cutting and neatly laminating the N layers of first biscuit without the film belts, sealing the first biscuit by using a PET vacuum packaging bag, and placing the sealed biscuit in an isostatic press under the pressure of 1-40MPa for static pressure for 5-40 minutes to form a second biscuit formed by fusing a plurality of layers of first biscuits, wherein the second biscuit is a GSPL-SNST silicon nitride casting biscuit; the multiple layers of biscuit blanks are fused by using an isostatic pressing machine, so that the biscuit blanks of each biscuit blank are almost completely consistent in performance when being sliced, the surface roughness of the GSPL-SNST silicon nitride casting biscuit is relatively small, and obvious layering and air hole phenomena are avoided.
The thickness of the second biscuit is T C Said T is C Also for customized substrate thickness, the calculation formula of the layer number N is
. And determining the required layer number N through a calculation formula according to the thickness of the substrate customized by the customer.
Preferably, the thickness of the first biscuit is preparedT 0 Is calculated by the formula
(ii) a Wherein a is the solid content (unit is%) determined according to GB/T17473.1-2008; />
And &>
Respectively the total mass of the anhydrous ethanol and the organic colloid,ffor adjusting the coefficients>
. The solid content (unit is%) determined by GB/T17473.1-2008 is convenient when in use, the mass ratio of the absolute ethyl alcohol in the prepared slurry to the organic colloid is convenient, and the thickness T of the first biscuit is manufactured according to the requirement 0 It can be determined by calculation, so that the required adjustment factor can be calculated. The slurry measured by GB/T17473.1-2008 has less mass which is 1g of slurry and needs to be weighed, and the waste of the pre-experiment process of the casting slurry caused by the adjustment coefficient of the adjusting equipment through the pre-experiment in the prior art is avoided. And the technical personnel who must be experienced in the prior art is not required to determine the approximate range of the adjusting coefficient firstly, and then tests are carried out in the range to determine the adjusting coefficient, so that the requirements on the experience of the technical personnel are low.
Preferably, the thickness of the first biscuitT 0 T calculated by the calculation formula 0 In mm.
Preferably, the SDPR pretreatment system is an inorganic solid powder pretreatment system for pretreating Si in the raw material 3 N 4 The powder and the inorganic sintering aid powder are subjected to pretreatment of drying and oxygen discharge;
the HVCM pretreatment system is an organic additive pretreatment system and is used for pretreating and mixing organic additives to prepare organic colloid;
the GSPL production line is a special silicon nitride tape-casting slurry production line and is used for mixing and grinding the pretreated inorganic solid and organic colloid to prepare micro-nano slurry. The micro-nano slurry produced by the special slurry production equipment ensures that the performance of a first biscuit produced by the casting of the micro-nano slurry is high.
The GSPL-SNST silicon nitride tape casting biscuit prepared by the preparation method has the surface roughness of the first biscuit and the second biscuit not more than 0.01 and no crack in any direction; meanwhile, on the cross section of the second biscuit, the variation coefficient of the density of the biscuit at different parts is not more than 0.001, and no obvious layering phenomenon and/or air hole phenomenon exist.
Compared with the prior art, the invention has the following beneficial effects: (1) The invention fuses a plurality of layers of biscuit blanks through the isostatic pressing machine, thus ensuring that the performance of each biscuit blank is almost completely consistent when the biscuit is sliced, the roughness of the produced GSPL-SNST silicon nitride casting biscuit is smaller, and no obvious layering and air hole phenomena exist, and ensuring the quality of the produced GSPL-SNST silicon nitride casting biscuit.
(2) The invention provides a calculation formula of the thickness of a first biscuit, wherein the solid content is measured through GB/T17473.1-2008 when the calculation formula is used, the mass ratio of the mass of absolute ethyl alcohol in prepared slurry to the mass of organic colloid is measured, and the thickness T of the first biscuit is manufactured according to the requirement 0 Can be determined by calculation, so that the required adjustment coefficient can be calculated; the solid content determined by GB/T17473.1-2008 needs to be weighed by the pulp with little mass, namely three 1g of pulp, so that the waste of the casting pulp pre-experiment process caused by adjusting the adjustment coefficient of equipment through pre-experiment in the prior art is avoided, and the approximate range of the adjustment coefficient is not needed to be determined by skilled technicians in the prior art, and then the experiment is carried out in the range to determine the adjustment coefficient, so that the requirement on the experience of the technicians is low.
(3) Before production, the inorganic solid and the organic additive are respectively pretreated by equipment and then mixed, so that the problems that in the prior art, various raw materials are directly mixed to prepare slurry, and the performance of the first blank generated by the production flow of the slurry prepared by an equipment production line is superior to that of the previous blank in all aspects are solved.
Detailed Description
In order to further understand the objects, structures, features and functions of the present invention, the following embodiments are described in detail.
Treating an inorganic solid raw material by an SDPR pretreatment system, treating an organic additive by an HVCM pretreatment system to generate an organic colloid, and mixing the organic colloid and the inorganic solid raw material by a GSPL production line to prepare GSPL-SNCS slurry 1 and slurry 2; m of slurry 1 Anhydrous ethanol /m Organic colloid 0.225, m of slurry 2 Anhydrous ethanol /m Organic colloid Is 0.45; both slurry 1 and slurry 2 had a solids content of 45% as determined by GB/T17473.1-2008.
Example 1
S1: preparation of a first biscuit:
the first biscuit thickness T is prepared 0 Is 0.01mm, will calculate the formula
Is deformed into
Will T 0 Solids content a of slurry 1, [ based on ] based on->
Substituting into the deformation formula to calculate the adjusting coefficient->
2, carrying out vacuum defoaming, tape casting and drying on the slurry 1 to form a first biscuit with the thickness of 0.01 mm;
s2: preparation of a second biscuit:
cutting and neatly laminating 32 layers of first biscuit after removing the film belts, sealing the first biscuit by using a PET vacuum packaging bag, and placing the sealed biscuit in an isostatic press for static pressure for 15 minutes under the pressure of 25MPa to form a second biscuit formed by fusing a plurality of layers of first biscuit, wherein the second biscuit is a GSPL-SNST silicon nitride casting biscuit, and the thickness of the second biscuit is 0.32mm; the surfaces of the first and second biscuits were visually observed to have no cracks in any direction, the surface roughness of the first biscuit produced was measured to be 0.00169 and the surface roughness of the second biscuit was measured to be 0.00161, respectively, the second biscuit was sliced, the variation coefficient of the density of the biscuit in the cross section of the second biscuit was measured to be 0.00031 by an instrument, and the surface roughness and the variation coefficient were recorded in table 1. The second biscuit obtained was observed under a microscope without significant delamination and/or porosity.
Example 2
S1: preparation of a first biscuit:
the first biscuit thickness T is prepared 0 Is 0.01mm, will calculate the formula
Is modified to that 0 Solids content a of slurry 1, [ based on ] based on->
Substituted into a transformation formula to calculate an adjustment factor->
2, carrying out vacuum defoaming, tape casting and drying on the slurry 1 to form a first biscuit with the thickness of 0.01 mm;
s2: preparation of a second biscuit:
cutting and neatly laminating 32 layers of the first biscuit after removing the film belts, sealing the first biscuit by using a PET vacuum packaging bag, and placing the sealed first biscuit in an isostatic press under the pressure of 25MPa for static pressure for 25 minutes to form a second biscuit formed by fusing a plurality of layers of the first biscuit, wherein the second biscuit is a GSPL-SNST silicon nitride casting biscuit, and the thickness of the second biscuit is 0.32mm; the surfaces of the first and second biscuits were visually observed to have no cracks in any direction, the surface roughness of the first biscuit produced was measured to be 0.00169 and the surface roughness of the second biscuit was measured to be 0.00142, respectively, the second biscuit was sliced, the variation coefficient of the density of the biscuit in the cross section of the second biscuit was measured to be 0.00025 by an instrument, and the surface roughness and the variation coefficient were recorded in table 1. The second biscuit obtained was observed under a microscope without significant delamination and/or porosity.
Example 3
S1: preparation of a first biscuit:
the first biscuit thickness T is prepared 0 Is 0.01mm, will calculate the formula
Is deformed into
Will T 0 Solids content a of syrup 1,. Beta.of syrup 1->
Substituting into the deformation formula to calculate the adjusting coefficient->
Is 2, slurry1, forming a first biscuit with the thickness of 0.01mm by vacuum defoaming, tape casting and drying;
s2: preparation of a second biscuit:
cutting and neatly laminating 32 layers of first biscuit after removing the film belts, sealing the first biscuit by using a PET vacuum packaging bag, and placing the sealed biscuit in an isostatic press under the pressure of 25MPa for static pressure for 35 minutes to form a second biscuit formed by fusing a plurality of layers of first biscuit, wherein the second biscuit is a GSPL-SNST silicon nitride casting biscuit, and the thickness of the second biscuit is 0.32mm; the surfaces of the first and second biscuits were visually observed to have no cracks in any direction, the surface roughness of the first biscuit produced was measured with an instrument to be 0.00169, the surface roughness of the second biscuit was measured to be 0.00123, the second biscuit was sliced, the coefficient of variation of the density of the biscuit in the cross section of the second biscuit was measured with an instrument to be 0.00021, and the surface roughness and the coefficient of variation were recorded in table 1. The second biscuit obtained was observed under a microscope without significant delamination and/or porosity.
Example 4
S1: preparation of a first biscuit:
the first biscuit thickness T is prepared 0 Is 0.02mm, will calculate the formula
Is deformed into
Will T 0 Solids content a of size 2,. Sup.4 of size 2 >>
Substituting into the deformation formula to calculate the adjusting coefficient->
2, carrying out vacuum defoaming, tape casting and drying on the slurry 2 to form a first biscuit with the thickness of 0.02 mm;
s2: preparation of a second biscuit:
cutting and neatly laminating 32 layers of first biscuit after removing the film belts, sealing the first biscuit by using a PET vacuum packaging bag, and placing the sealed biscuit in an isostatic press for static pressure for 15 minutes under the pressure of 25MPa to form a second biscuit formed by fusing a plurality of layers of first biscuit, wherein the second biscuit is a GSPL-SNST silicon nitride casting biscuit, and the thickness of the second biscuit is 0.64mm; the surfaces of the first and second biscuits were visually observed to have no cracks in any direction, the surface roughness of the first biscuit produced was measured to be 0.00194 and the surface roughness of the second biscuit was measured to be 0.00186, respectively, the second biscuit was sliced, the variation coefficient of the density of the biscuit in the cross section of the second biscuit was measured to be 0.00055 by an instrument, and the surface roughness and the variation coefficient were recorded in table 1. The second biscuit obtained was observed under a microscope without significant delamination and/or porosity.
Example 5
S1: preparation of a first biscuit:
the first biscuit thickness T is prepared 0 At 0.02mm, the calculation formula
Is deformed into->
Will T 0 Solids content a of size 2,. Sup.4 of size 2 >>
Substituting into the deformation formula to calculate the adjusting coefficient->
2, carrying out vacuum defoaming, tape casting and drying on the slurry 2 to form a first biscuit with the thickness of 0.02 mm;
s2: preparation of a second biscuit:
cutting and neatly laminating 32 layers of first biscuit after removing the film belts, sealing the first biscuit by using a PET vacuum packaging bag, and placing the sealed biscuit in an isostatic press under the pressure of 25MPa for static pressure for 25 minutes to form a second biscuit formed by fusing a plurality of layers of first biscuit, wherein the second biscuit is a GSPL-SNST silicon nitride casting biscuit, and the thickness of the second biscuit is 0.64mm; the surfaces of the first and second biscuits were visually observed to have no cracks in any direction, the surface roughness of the first biscuit produced was measured with an instrument to be 0.00194, the surface roughness of the second biscuit was measured to be 0.00174, the second biscuit was sliced, the coefficient of variation of the density of the biscuit in the cross section of the second biscuit was measured with an instrument to be 0.00047, and the surface roughness and the coefficient of variation were recorded in table 1. The second biscuit obtained was observed under a microscope without significant delamination and/or porosity.
Example 6
S1: preparation of a first biscuit:
the first biscuit thickness T is prepared 0 Is 0.02mm, will calculate the formula
Is deformed into
Will T 0 Solids content a of size 2,. Sup.4 of size 2 >>
Substituted into a transformation formula to calculate an adjustment factor->
2, carrying out vacuum defoaming, tape casting and drying on the slurry 2 to form a first biscuit with the thickness of 0.02 mm;
s2: preparation of a second biscuit:
cutting and neatly laminating 32 layers of first biscuit after film belts are removed, sealing the first biscuit by using a PET vacuum packaging bag, and placing the first biscuit in an isostatic press under the pressure of 25MPa for static pressure for 35 minutes to form a second biscuit formed by fusing a plurality of layers of first biscuits, wherein the second biscuit is a GSPL-SNST silicon nitride casting biscuit, and the thickness of the second biscuit is 0.64mm; the surfaces of the first and second biscuits were visually observed to have no cracks in any direction, the surface roughness of the first biscuit produced was measured to be 0.00194 and the surface roughness of the second biscuit was measured to be 0.00163, respectively, the second biscuit was sliced, the variation coefficient of the density of the biscuit in the cross section of the second biscuit was measured to be 0.00033 by an instrument, and the surface roughness and the variation coefficient were recorded in table 1. The second biscuit obtained was observed under a microscope without significant delamination and/or porosity.
According to the table, when the pulp is usedThe thickness T of the first biscuit is determined when the solid content of the material and the adjustment coefficient of the equipment are determined 0 With m Anhydrous ethanol /m Organic colloid Increases with increasing ratio of (d); when the isostatic pressing pressure is the same, the surface roughness of the second biscuit with the same thickness is gradually reduced along with the prolonging of the isostatic pressing time, and the density variation coefficient of the transverse section of the second biscuit is also gradually reduced. From a comparison of slurry 1 and slurry 2, it is clear that the coefficient of variation of the surface roughness of the second biscuit and the density of the second biscuit cross section both increase with increasing thickness of the first biscuit under the same static pressure condition.
The present invention has been described in relation to the above embodiments, which are only exemplary of the implementation of the present invention. It should be noted that the disclosed embodiments do not limit the scope of the invention. Rather, it is intended that the invention be covered by the appended claims without departing from the spirit and scope of the invention.
Claims (3)
1. The preparation method of the GSPL-SNST silicon nitride tape casting biscuit is characterized by comprising the following steps: the method comprises the following steps:
s1: preparation of a first biscuit:
treating inorganic solid with SDPR pretreatment system, treating organic additive with HVCM pretreatment system to obtain organic colloid, mixing the organic colloid with GSPL production line to obtain GSPL-SNCS slurry, vacuum defoaming, casting, and drying to obtain GSPL-SNCS slurry with thickness ofT 0 A first biscuit of (a);
the inorganic solid at least comprises Si 3 N 4 Powder and inorganic sintering aid powder;
the organic colloid at least comprises a mixture of castor oil, absolute ethyl alcohol, polymethacrylene, polyethylene glycol and glycerol monooleate;
s2: preparation of a second biscuit:
cutting and neatly stacking the N layers of first biscuit without the film belts, sealing the first biscuit by using a PET vacuum packaging bag, and placing the sealed first biscuit in an isostatic press under the pressure of 1-40MPa for static pressure for 5-40 minutes to form a second biscuit formed by fusing a plurality of layers of first biscuits, wherein the second biscuit is a GSPL-SNST silicon nitride casting biscuit;
the thickness of the second biscuit is T C Said T is C Also for customized substrate thickness, the calculation formula of the layer number N is
(ii) a Preparing the thickness of the first biscuitT 0 Is calculated as->
(ii) a Wherein a is the solid content (unit is%) of the GSPL-SNCS sizing agent determined according to GB/T17473.1-2008; />
And &>
Respectively the total mass of the absolute ethyl alcohol and the organic colloid,ffor adjusting the coefficient>
；
The SDPR pretreatment system is an inorganic solid powder pretreatment system and is used for pretreating Si in the raw material 3 N 4 The powder and the inorganic sintering aid powder are subjected to pretreatment of drying and oxygen discharge;
the HVCM pretreatment system is an organic additive pretreatment system and is used for pretreating and mixing organic additives to prepare organic colloid;
the GSPL production line is a special silicon nitride tape-casting slurry production line and is used for mixing and grinding the pretreated inorganic solid and organic colloid to prepare micro-nano slurry.
2. A method of making a GSPL-SNST silicon nitride cast biscuit according to claim 1, wherein: of the first biscuitThickness ofT 0 T calculated by the calculation formula 0 In mm.
3. The GSPL-SNST silicon nitride cast biscuit prepared by the preparation method of claim 1, characterized in that: the surface roughness of the first biscuit and the second biscuit is not more than 0.01 mu m, and no crack exists in any direction; meanwhile, on the cross section of the second biscuit, the variation coefficient of the density of the biscuit at different parts is not more than 0.001, and no obvious layering phenomenon and/or air hole phenomenon exist.
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