CN112850733B - HTCC packaging tube shell glass pigment, preparation method and application - Google Patents

HTCC packaging tube shell glass pigment, preparation method and application Download PDF

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CN112850733B
CN112850733B CN202110226284.6A CN202110226284A CN112850733B CN 112850733 B CN112850733 B CN 112850733B CN 202110226284 A CN202110226284 A CN 202110226284A CN 112850733 B CN112850733 B CN 112850733B
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cyclodextrin
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gel
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CN112850733A (en
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李生
邵训达
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Jiangsu Yixing Electronic Device General Factory Co ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0009Pigments for ceramics
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L23/00Details of semiconductor or other solid state devices
    • H01L23/02Containers; Seals
    • H01L23/06Containers; Seals characterised by the material of the container or its electrical properties
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/36Glass starting materials for making ceramics, e.g. silica glass
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/602Making the green bodies or pre-forms by moulding
    • C04B2235/6025Tape casting, e.g. with a doctor blade
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9646Optical properties
    • C04B2235/9661Colour

Abstract

The invention discloses an HTCC packaging tube shell glass pigment, which comprises the following inorganic powder raw materials in parts by weight: 20-32 parts of aluminum oxide, 15-22 parts of kaolin, 16-20 parts of talcum powder, 8-13 parts of molybdenum trioxide, 6-12 parts of chromium oxide, 5-14 parts of calcium carbonate and 1-6 parts of interconnecting agent. Compared with the HTCC packaging tube shell prepared by conventional ingredients, the invention has the following advantages: the glass pigment prefabrication method can obviously reduce pulping viscosity, reduce pulping difficulty and facilitate large-scale production; the glass pigment has deeper porcelain color and obviously improves the porcelain density and the porcelain bending resistance.

Description

HTCC packaging tube shell glass pigment, preparation method and application
Technical Field
The invention relates to the technical field of ceramics for packaging microelectronic components, in particular to an HTCC packaging tube shell glass pigment, a preparation method and application thereof.
Background
The black alumina ceramic package tube has a series of excellent performances of light shielding property, good air tightness, strong radiation resistance, high strength, high hardness, abrasion resistance, high temperature resistance, good insulativity, acid and alkali resistance and the like, and is widely applied to integrated circuit package. With the development of microelectronics and semiconductor industry to high density and high integration, the requirements on the strength, the air tightness and the circuit design density of ceramic package shells are higher. The traditional method for preparing the tube shell is an HTCC process, namely a high-temperature co-firing ceramic process, and the related flow is to prepare casting slurry by 65-68% of alumina, 8-10% of fluxing agent auxiliary materials and colorant auxiliary materials and 20-25% of casting auxiliary materials, and then cut, print, laminate, hot press, co-firing, electroplating and other working procedures are carried out on the cast membrane. The proportioning mode has the advantages that as the auxiliary materials are too much and the fluctuation of the specific surface area is too large, the slurry with high solid content is difficult to prepare when the casting slurry is prepared, and great inconvenience is brought to factory production; and the density of the front and back surfaces of the prepared diaphragm is uneven, and the pigment is easy to segregate on the surface, thus causing interference to the design of a printed circuit of a product.
Under the condition that the alumina content of the HTCC packaging tube shell porcelain body is not more than 92%, fine tillage and fine work of a ceramic preparation technology are needed to be realized to ensure the improvement of the overall performance of the ceramic tube shell, such as adopting alumina powder and auxiliary materials with finer particles, adopting a more scientific ceramic formula, carrying out particle grading on the powder, carrying out advanced pretreatment on auxiliary materials of a cosolvent to prepare microcrystalline glass and the like, but the method does not essentially solve the problems of uneven density of the upper surface and the lower surface of a casting film, segregation of pigment, large pulping difficulty in large-scale production, excessively high cofiring temperature and the like; based on the above, the invention provides an HTCC packaging shell glass pigment.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an HTCC packaging tube shell glass pigment, a preparation method and application thereof.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides an HTCC packaging tube shell glass pigment, which comprises the following inorganic powder raw materials in parts by weight:
20-32 parts of aluminum oxide, 15-22 parts of kaolin, 16-20 parts of talcum powder, 8-13 parts of molybdenum trioxide, 6-12 parts of chromium oxide, 5-14 parts of calcium carbonate and 1-6 parts of interconnecting agent;
the inorganic powder raw materials firstly undergo a gelation reaction, and the gelation raw materials comprise: 2.0 to 2.5 parts of acrylamide organic monomer, 0.1 to 0.12 part of N, N' -methylene bisacryloyl cross-linking agent, 0.5 to 1.0 part of Rongmen Has OROTAN 1124 dispersant, 0.2 to 0.4 part of ammonium persulfate initiator, 0.05 to 0.1 part of tetramethyl ethylenediamine, 10 to 15ml of 28 percent ammonia water solution and 40 to 50 parts of deionized water;
the preparation method of the interconnection agent comprises the following steps:
s1: the cyclodextrin is sent into a fatty alcohol polyoxyethylene ether sodium sulfate solution with the mass fraction of 10-30% to be stirred for 20-30min at a low speed, the stirring rotation speed is 100-200r/min, the stirring is finished, then the cyclodextrin is taken out and washed, the cyclodextrin is sent into a proton irradiation box to be irradiated, the irradiation power is 300-500W, the irradiation time is 10-20min, the active cyclodextrin is obtained after the irradiation is finished, then the cyclodextrin is sent into a silane coupling agent to be subjected to ultrasonic reaction for 1-2h, the ultrasonic power is 200-300W, the reaction temperature is 100-120 ℃, and the amphoteric cyclodextrin is obtained after the reaction is finished;
s2: sending graphene into an acetone solvent to be stirred for 10-20min, wherein the stirring speed is 100-150r/min, then adding modified bentonite to perform ultrasonic dispersion for 20-30min, the ultrasonic power is 300-500W, and the ultrasonic is finished to obtain graphene liquid;
s3: and (3) sending the amphoteric cyclodextrin into graphene liquid for reaction treatment, wherein the reaction temperature is 85-95 ℃, the reaction time is 20-30min, and the interconnecting agent is obtained after the reaction is finished.
Preferably, the modified bentonite is obtained by hot-pressing bentonite at 800-1200 ℃ for 20-30min under the hot-pressing pressure of 10-20 MPa.
Preferably, the gelation reaction mixes and fully ball-mills the inorganic powder raw material and the gel raw material, the particle size of all the powder materials is controlled to be d50=3-5 mu m, the formed gel slurry suspension is stable and uniform, the speed of the gelation reaction is controlled to form a wet blank, and the wet blank is dried to prepare a gel block.
Preferably, the gel block is calcined at 1200-1400 deg.c and in weak oxygen atmosphere for 2-4 hr to react fully.
Preferably, the calcined gel block is jaw-crushed to a particle size of 1-3 mm, wet-ground by a sand mill until the particle D50=0.5-0.8 μm, oven-dried at 100-150 ℃ and screened by a stainless steel mesh sieve with 100 meshes to prepare Al 2 O 3 -MgO-CaO-SiO 2 -MoO 3 -Cr 2 O 3 Composite spinel.
The invention provides an HTCC packaging tube shell glass pigment, which comprises the following steps:
(1) Preparing and ball-milling inorganic powder gel slurry to enable the particle size of inorganic powder particles to reach D50=3-5 mu m;
(2) Triggering a gel reaction to form an inorganic powder into a gel block, and calcining the block in a weak oxygen atmosphere to synthesize a complex-phase spinel;
(3) Jaw crushing, wet sand grinding, stoving and sieving to obtain glass pigment of 0.5-0.8 micron size.
The invention also provides a glass pigment which is prepared from 65 to 68 percent of alumina, 8 to 10 percent of glass pigment and 20 to 25 percent of casting auxiliary agent by pulping, casting, punching, printing, lamination, cutting, sintering, brazing and electroplating, and the black alumina HTCC integrated circuit ceramic package shell, crystal oscillator, MEMS sensor package substrate, image sensor package shell and black alumina substrate are prepared, wherein the cofiring temperature is 1540 to 1580 ℃.
Compared with the prior art, the invention has the following beneficial effects:
compared with the conventional preparation method for preparing the HTCC packaging tube shell, the method for prefabricating the glass pigment can obviously reduce the pulping viscosity, reduce the pulping difficulty and facilitate large-scale production; the porcelain color of the glass pigment is deeper, and the improvement on the porcelain density and the porcelain bending resistance is very obvious; meanwhile, the preparation method of the prefabricated glass pigment is simpler in material mixing, the sintering temperature is lower than that of the common HTCC packaging tube shell, and the energy-saving and emission-reducing effects are better;
the introduced interconnecting agent is subjected to improved treatment by adopting cyclodextrin, the cyclodextrin has the dual properties of organophilic and inorganic, firstly, the cyclodextrin is subjected to inorganic activation, then the amphoteric property of the cyclodextrin is enhanced by coupling organic treatment, then the cyclodextrin and graphene are subjected to co-coupling treatment, the bentonite subjected to hot-pressing calcination is added in the reprocessing of the graphene, the lamellar structure of the bentonite is shrunk, so that the shrinkage degree of the graphene is improved, and after the bentonite reacts with the interconnecting agent, the gel raw materials are interconnected by accessing inorganic powder, the reaction degree between the raw materials is enhanced, and then the gelation reaction is improved, and the performance of the glass pigment is improved.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The HTCC packaging shell glass pigment comprises the following inorganic powder raw materials in parts by weight:
20-32 parts of aluminum oxide, 15-22 parts of kaolin, 16-20 parts of talcum powder, 8-13 parts of molybdenum trioxide, 6-12 parts of chromium oxide, 5-14 parts of calcium carbonate and 1-6 parts of interconnecting agent;
the inorganic powder raw materials firstly undergo a gelation reaction, and the gelation raw materials comprise: 2.0 to 2.5 parts of acrylamide organic monomer, 0.1 to 0.12 part of N, N' -methylene bisacryloyl cross-linking agent, 0.5 to 1.0 part of Rongmen Has OROTAN 1124 dispersant, 0.2 to 0.4 part of ammonium persulfate initiator, 0.05 to 0.1 part of tetramethyl ethylenediamine, 10 to 15ml of 28 percent ammonia water solution and 40 to 50 parts of deionized water;
the preparation method of the interconnection agent comprises the following steps:
s1: the cyclodextrin is sent into a fatty alcohol polyoxyethylene ether sodium sulfate solution with the mass fraction of 10-30% to be stirred for 20-30min at a low speed, the stirring rotation speed is 100-200r/min, the stirring is finished, then the cyclodextrin is taken out and washed, the cyclodextrin is sent into a proton irradiation box to be irradiated, the irradiation power is 300-500W, the irradiation time is 10-20min, the active cyclodextrin is obtained after the irradiation is finished, then the cyclodextrin is sent into a silane coupling agent to be subjected to ultrasonic reaction for 1-2h, the ultrasonic power is 200-300W, the reaction temperature is 100-120 ℃, and the amphoteric cyclodextrin is obtained after the reaction is finished;
s2: sending graphene into an acetone solvent to be stirred for 10-20min, wherein the stirring speed is 100-150r/min, then adding modified bentonite to perform ultrasonic dispersion for 20-30min, the ultrasonic power is 300-500W, and the ultrasonic is finished to obtain graphene liquid;
s3: and (3) sending the amphoteric cyclodextrin into graphene liquid for reaction treatment, wherein the reaction temperature is 85-95 ℃, the reaction time is 20-30min, and the interconnecting agent is obtained after the reaction is finished.
The modified bentonite of the embodiment is prepared by carrying out hot pressing reaction on bentonite at 800-1200 ℃ for 20-30min under the hot pressing pressure of 10-20 MPa.
The gelation reaction of this example mixes and fully ball-mills the inorganic powder raw material and the gel raw material, the particle size of all the powder is controlled to d50=3-5 μm, the formed gel slurry suspension is stable and uniform, the speed of the gelation reaction is controlled to form a wet blank, and the wet blank is dried to prepare a gel block.
The gel block of this example was calcined at 1200-1400 deg.c in a weak oxygen atmosphere for 2-4 hours to allow sufficient reaction between the oxide elements.
The calcined gel block of this example was jaw-crushed to a particle size of 1 to 3mm, wet-milled with a sand mill to a particle d50=0.5 to 0.8 μm, oven-dried at 100 to 150 ℃, and screened through a 100 mesh stainless steel screen to produce Al 2 O 3 -MgO-CaO-SiO 2 -MoO 3 -Cr 2 O 3 Composite spinel.
The preparation process of the HTCC packaging shell glass pigment comprises the following steps of:
(1) Preparing and ball-milling inorganic powder gel slurry to enable the particle size of inorganic powder particles to reach D50=3-5 mu m;
(2) Triggering a gel reaction to form an inorganic powder into a gel block, and calcining the block in a weak oxygen atmosphere to synthesize a complex-phase spinel;
(3) Jaw crushing, wet sand grinding, stoving and sieving to obtain glass pigment of 0.5-0.8 micron size.
The glass pigment is prepared from 65-68% of alumina, 8-10% of glass pigment and 20-25% of casting auxiliary agent by pulping, casting, punching, printing, lamination, cutting, sintering, brazing and electroplating to prepare a black alumina HTCC integrated circuit ceramic package shell, a crystal oscillator, a MEMS sensor package substrate, an image sensor package shell and a black alumina substrate, wherein the cofiring temperature is 1540-1580 ℃.
Example 1
The preparation process of the HTCC packaging shell glass pigment comprises the following steps: (1) Preparing and ball-milling inorganic powder gel slurry to enable the particle size of inorganic powder particles to reach D50=4μm; (2) Triggering a gel reaction to form an inorganic powder into a gel block, and calcining the block in a weak oxygen atmosphere to synthesize a complex-phase spinel; (3) The sintered complex spinel is subjected to jaw crushing, wet sanding, drying and sieving treatment to obtain the glass pigment with the particle size of 0.6 mu m.
The inorganic powder raw materials comprise: 28 parts of aluminum oxide, 18 parts of kaolin, 18 parts of talcum powder, 10 parts of molybdenum trioxide, 12 parts of chromium oxide, 8 parts of calcium carbonate and 1 part of interconnecting agent.
The preparation method of the interconnection agent of the embodiment comprises the following steps:
s1: the method comprises the steps of (1) feeding cyclodextrin into a 10% mass fraction fatty alcohol polyoxyethylene ether sodium sulfate solution, stirring for 20min at a low speed, wherein the stirring speed is 100r/min, stirring is finished, then taking out, washing with water, feeding into a proton irradiation box, carrying out irradiation treatment, wherein the irradiation power is 300W, the irradiation time is 10min, obtaining active cyclodextrin, feeding into a silane coupling agent, carrying out ultrasonic reaction for 1h, the ultrasonic power is 200W, the reaction temperature is 100 ℃, and finishing the reaction to obtain amphoteric cyclodextrin;
s2: feeding graphene into an acetone solvent, stirring for 10min at a stirring speed of 100r/min, then adding modified bentonite, performing ultrasonic dispersion for 20min, wherein the ultrasonic power is 300W, and ending ultrasonic treatment to obtain graphene liquid;
s3: and (3) sending the amphoteric cyclodextrin into graphene liquid for reaction treatment, wherein the reaction temperature is 85 ℃, the reaction time is 20min, and the reaction is finished to obtain the interconnecting agent.
The modified bentonite of the embodiment is prepared by carrying out hot pressing reaction on bentonite at 800 ℃ for 20min under the hot pressing pressure of 10 MPa.
The gel raw materials comprise: 2.2 parts of organic monomer (acrylamide), 0.1 part of cross-linking agent (N, N' -methylene bisacrylamide), 0.8 part of dispersing agent (Rogowski OROTAN 1124), 0.2 part of initiator (ammonium persulfate), 0.07 part of catalyst (tetramethyl ethylenediamine), 12ml of PH regulator (28% ammonia solution) and 43 parts of deionized water.
The gelation process is to weigh inorganic powder, mix and ball mill the inorganic powder with gel raw material, control the speed of the gel reaction to form wet blank, and dry the wet blank to prepare gel block.
Calcining the gel block at 1250 deg.c in weak oxygen atmosphere for 2 hr to react fully.
Crushing the calcined material blocks in a jaw crusher to obtain particles with the size of 1mm, wet-grinding the particles in a sand mill to obtain slurry with the particle D50=0.6 mu m, pouring the slurry into a 100-150 ℃ oven for drying, and sieving with a 100-mesh stainless steel screen to obtain Al 2 O 3 -MgO-CaO-SiO 2 -MoO 3 -Cr 2 O 3 Composite spinel, labeled glass colorant (1).
The method for preparing the ceramic package tube shell material by using the glass pigment in the embodiment comprises the following steps: 67.69% of alumina, 9.23% of glass pigment (1) and 23.08% of casting auxiliary agent are prepared into casting slurry powder, and then uniformly mixed and cast into a mold.

Claims (4)

1. The HTCC packaging shell glass pigment is characterized in that the inorganic powder raw materials of the glass pigment comprise the following raw materials in parts by weight:
20-32 parts of aluminum oxide, 15-22 parts of kaolin, 16-20 parts of talcum powder, 8-13 parts of molybdenum trioxide, 6-12 parts of chromium oxide, 5-14 parts of calcium carbonate and 1-6 parts of interconnecting agent;
the inorganic powder raw materials firstly undergo a gelation reaction, and the gelation raw materials comprise: 2.0 to 2.5 parts of acrylamide organic monomer, 0.1 to 0.12 part of N, N' -methylene bisacryloyl cross-linking agent, 0.5 to 1.0 part of Rongmen Has OROTAN 1124 dispersant, 0.2 to 0.4 part of ammonium persulfate initiator, 0.05 to 0.1 part of tetramethyl ethylenediamine, 10 to 15ml of 28 percent ammonia water solution and 40 to 50 parts of deionized water;
the preparation method of the interconnection agent comprises the following steps:
s1: the cyclodextrin is sent into a fatty alcohol polyoxyethylene ether sodium sulfate solution with the mass fraction of 10-30% to be stirred for 20-30min at a low speed, the stirring rotation speed is 100-200r/min, the stirring is finished, then the cyclodextrin is taken out and washed, the cyclodextrin is sent into a proton irradiation box to be irradiated, the irradiation power is 300-500W, the irradiation time is 10-20min, the active cyclodextrin is obtained after the irradiation is finished, then the cyclodextrin is sent into a silane coupling agent to be subjected to ultrasonic reaction for 1-2h, the ultrasonic power is 200-300W, the reaction temperature is 100-120 ℃, and the amphoteric cyclodextrin is obtained after the reaction is finished;
s2: sending graphene into an acetone solvent to be stirred for 10-20min, wherein the stirring speed is 100-150r/min, then adding modified bentonite to perform ultrasonic dispersion for 20-30min, the ultrasonic power is 300-500W, and the ultrasonic is finished to obtain graphene liquid;
s3: the amphoteric cyclodextrin is sent into the graphene liquid for reaction treatment, the reaction temperature is 85-95 ℃, the reaction time is 20-30min, and the interconnecting agent is obtained after the reaction is finished;
the gelation reaction is to mix and fully ball mill inorganic powder raw materials and gel raw materials, the particle size of all the powder materials is controlled to D50=3-5 mu m, the formed gel slurry suspension is stable and uniform, the speed of the gelation reaction is controlled to form wet blanks, and the wet blanks are dried to prepare gel blocks;
the gel block is calcined at 1200-1400 deg.c and weak oxygen atmosphere for 2-4 hr to react fully.
2. The HTCC packaging shell glass pigment of claim 1, wherein the modified bentonite is obtained by hot pressing bentonite at 800-1200 ℃ for 20-30min under a hot pressing pressure of 10-20 MPa.
3. The HTCC package tube glass colorant according to claim 1, wherein the calcined gel block is jaw-crushed to a particle size of 1-3 mm, wet-milled by a sand mill to a particle d50=0.5-0.8 μm, oven-dried at 100-150 ℃, and screened through a 100 mesh stainless steel screen to make Al 2 O 3 -MgO-CaO-SiO 2 -MoO 3 -Cr 2 O 3 Composite spinel.
4. A HTCC package casing glass colorant according to any one of claims 1-3, wherein the preparation process comprises the steps of:
(1) Preparing and ball-milling inorganic powder gel slurry to enable the particle size of inorganic powder particles to reach D50=3-5 mu m;
(2) Triggering a gel reaction to form an inorganic powder into a gel block, and calcining the block in a weak oxygen atmosphere to synthesize a complex-phase spinel;
(3) Jaw crushing, wet sand grinding, stoving and sieving to obtain glass pigment of 0.5-0.8 micron size.
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