CN102515848A - Black pigment for electronic packaging ceramic and preparation method thereof - Google Patents

Black pigment for electronic packaging ceramic and preparation method thereof Download PDF

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Publication number
CN102515848A
CN102515848A CN2011104175923A CN201110417592A CN102515848A CN 102515848 A CN102515848 A CN 102515848A CN 2011104175923 A CN2011104175923 A CN 2011104175923A CN 201110417592 A CN201110417592 A CN 201110417592A CN 102515848 A CN102515848 A CN 102515848A
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ball
black pigment
abrading
preparation
electronic packaging
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CN102515848B (en
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徐雷
赵康
汤玉斐
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Xian University of Technology
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Xian University of Technology
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Abstract

The invention discloses a black pigment for electronic packaging ceramic. The black pigment comprises raw materials of Fe2O3, Cr2O3, MnCO3, CoO, SiO2, TiO2 and MgO according to certain weight percentages. The invention also discloses a preparation method of the black pigment. The preparation method concretely comprises the following steps: respectively cleaning solid materials of the raw materials, respectively screening the solid materials by a screen mesh, respectively drying the solid materials, weighing needed raw materials, mixing the raw materials, ball-milling, drying, sintering at a high temperature, crushing, screening by the screen mesh, ball-milling again, and drying. The black pigment for the electronic packaging ceramic of the invention makes the packaging ceramic be black and have the light proofness, and does not influence heat, strength and insulation packaging requirements of the packaging ceramic. Steps of the preparation method of the invention are simple, so the preparation method is easy to realize.

Description

A kind of Electronic Packaging pottery is with black pigment and preparation method thereof
Technical field
The invention belongs to electronic ceramics packaged material technical field, be specifically related to a kind of Electronic Packaging pottery and use black pigment, the invention still further relates to the preparation method of this Electronic Packaging pottery with black pigment.
Background technology
Electronic package material is a kind ofly to be used to carry electronic devices and components, to guarantee the material that circuit connects and has over-all propertieies such as good electrical insulativity, thermal conductivity, requires packaged material and packed components and parts to have good matching at aspects such as electricity, physics and chemical properties.Stupalith is a kind of as packaged material, because of its special performances is used more and more widely.The salient features of stupalith comprises: good heat-conducting; High insulating property have close linear expansivity with components and parts, excellent high frequency characteristics; Over-all propertieies such as stable chemical performance are widely used in the encapsulation and the multi-layer stacks ceramic substrate of unicircuit, multicore sheet module.Ceramic packaging material commonly used mainly contains Al 2O 3, AlN, SiC, BN and BeO etc.
High speed development along with electronic technology; Electronic component is to chip type, miniaturized, high integration development, and is increasingly high to the precision requirement of unicircuit, therefore also increasingly high to the requirement of packaged material; And encapsulate the size that can reduce components and parts significantly with stupalith; The tolerance range and the sensitivity that can improve circuit simultaneously can make 30～100 times of volume-diminished like the quartz oscillator that adopts the stupalith encapsulation, and corresponding precision and stability improve significantly.But, for SIC and some electronic products (like quartz resonator, charactron liner plate etc.), having tangible photosensitivity, traditional packaged material can not meet the demands, and therefore requires packaged material to have certain opacifying property.Can change its color through in stupalith, adding an amount of colorant, can make packaging ceramic present black, make it have certain light absorption, thereby guarantee the pinpoint accuracy and the susceptibility of electronic component and add black pigment.Black pigment is the important component part of packaging ceramic, and what determining packaged material finally is chromatic effect and other correlated performance.Traditional pottery mainly contains two types of application with black pigment: glaze is used and base usefulness, like domestic ceramics, encaustic brick, decorative porcelain etc., is then rarely having report aspect the Electronic Packaging pottery.Use colorant as the packaging ceramic material, except considering painted effect, also will guarantee other character that packaged material should have, like high insulativity, physical strength, thermal property etc.
Summary of the invention
The purpose of this invention is to provide a kind of Electronic Packaging pottery and use black pigment, can make packaging ceramic present black, make packaging ceramic have opacifying property, and do not influence calorifics, intensity and the insulativity encapsulation requirement of packaging ceramic.
Another object of the present invention provides the preparation method of this Electronic Packaging pottery with black pigment, and step is simple, realizes easily.
The technical scheme that the present invention adopted is that a kind of Electronic Packaging pottery is used black pigment, it is characterized in that, according to weight percent, is made up of following feed composition: Fe 2O 320%～30%, Cr 2O 330%～35%, MnCO 325%～35%, CoO 0%～5%, SiO 21%～2%, TiO 21.5%～2.5%, MgO 0.5%～2.5%, more than each weight percentages of components sum be 100%.
Another technical scheme that the present invention adopted is that a kind of Electronic Packaging pottery is characterized in that with the preparation method of black pigment concrete steps are following:
Step 1, with Fe 2O 3, Cr 2O 3, MnCO 3, CoO, SiO 2, TiO 2, the MgO solid material puts into solvent respectively and cleans at Ultrasonic Cleaners, the raw material after cleaning is crossed screen cloth respectively after, place the loft drier inner drying;
In step 2, the raw material that in step 1, obtains, take by weighing respectively according to weight percent: Fe 2O 320%～30%, Cr 2O 330%～35%, MnCO 325%～35%, CoO 0%～5%, SiO 21%～2%, TiO 21.5%～2.5%, MgO 0.5%～2.5%, more than each weight percentages of components sum be 100%;
After step 3, the raw materials mix that step 2 is taken by weighing, add an amount of solvent, place ball mill ball-milling processing 4h～10h;
Step 4: the material that step 3 obtains is put into loft drier, dry 1h～3h under 100 ℃～120 ℃ temperature;
Step 5: the material that step 4 is obtained places crucible, is heated to 1200 ℃～1350 ℃ in the high temperature sintering furnace, insulation 1h～2h;
Step 6: after the material that obtains in the step 5 pulverized, cross 300 eye mesh screens, add an amount of solvent, place ball mill ball-milling processing 3h～5h;
Step 7: the material that step 6 obtains is put into loft drier, and dry 1h～3h under 100 ℃～120 ℃ temperature promptly makes.
In the step 1, the ultrasonic cleaning number of times is 1～2 time, and each scavenging period is 10min～30min.
In step 1, step 3 and the step 6, employed solvent is pure water, ethanol, acetone or toluene.
In step 3 and the step 6; During ball-milling processing; Institute uses ball mill to be planetary ball mill; The ball grinder that uses be corundum ceramic ball grinder, zirconia ceramics ball grinder, aluminium nitride ceramics ball grinder, nylon ball grinder or urethane ball grinder, the abrading-ball that uses be corundum ceramic abrading-ball, zirconia ceramics abrading-ball, aluminium nitride ceramics abrading-ball or agate abrading-ball.
Electronic Packaging pottery of the present invention has the following advantages with black pigment:
1, is widely used, can be used for all kinds of packaging ceramics, like aluminum oxide, zirconium white, aluminium nitride AlN, silicon nitride packaging ceramic etc.
2, through in the packaging ceramic material, adding this an amount of black pigment, carry out sintering after, can make packaging ceramic present black, make it have absorptivity, thereby guarantee the pinpoint accuracy and the susceptibility of electronic component light.
3, in the packaging ceramic material, behind this colorant of interpolation, both can under atmospheric condition, also can carry out sintering in a vacuum.
4, high-temperature stability is good, and the packaging ceramic that adds this colorant can carry out sintering (900 ℃～1400 ℃) under bigger TR and higher temperature, has the good chromatic effect and not volatile that is.
5, add the packaging ceramic of black pigment, on physical and chemical performance,, all meet the requirement of packaging ceramic like insulativity, physical strength, dielectricity, heat conductivity etc.
The black pigment epigranular of preparing method's preparation of the present invention, step is simple, realizes easily.
Description of drawings
Fig. 1 is the ceramic x x ray diffration pattern x with black pigment of Electronic Packaging that the embodiment of the invention 2 makes;
Fig. 2 be the Electronic Packaging pottery that makes of the embodiment of the invention 3 with black pigment electron scanning micrograph.
Fig. 3 is added with Electronic Packaging pottery that the embodiment of the invention 3 the makes electron scanning micrograph with the aluminum oxide packaging ceramic substrate of black pigment.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
A kind of Electronic Packaging pottery of the present invention, is made up of following feed composition: Fe according to weight percent with black pigment and preparation method thereof 2 O 320%～30%, Cr 2O 330%～35%, MnCO 325%～35%, CoO 0%～5%, SiO 21%～2%, TiO 21.5%～2.5%, MgO 0.5%～2.5%, more than each weight percentages of components sum be 100%.
Fe 2O 3, Cr 2O 3, MnCO 3(the calcining back is MnO), CoO and TiO 2Be painted oxidation material, in sintering process, have the part volatilization usually, and behind high temperature sintering, can form dissimilar compounds, can effectively reduce the volatility of prepared black pigment, guarantee the good chromatic effect that is with spinel structure.In addition, the MnCO in the coloring oxide 3And TiO 2In the alumina-ceramic sintering process, can reduce the sintering temperature of alumina-ceramic.This is because TiO 2, MnO lattice parameter and Al 2O 3Close, and be valence variation element, can with Al 2O 3Form dissimilar sosoloid, this effect of appraising at the current rate has increased Al 2O 3Lattice imperfection, activation lattice, thereby reduced sintering temperature.Moreover, SiO 2, MgO is that glass forms phase, in the sintering process of Electronic Packaging pottery with black pigment, the generation of glassy phase can suppress the volatilization of colorant, the while also can suitably be reduced the firing temperature of stupalith.MgO in sintering process, also can with Fe 2O 3, Cr 2O 3, painted oxide compound such as MnO interacts, and forms complicated more spinel compound, can suppress the volatilization of black pigment.
Mn in the black pigment of the present invention's preparation 2+, Fe 3+, Cr 3+Deng the transition metal that is the fourth phase in the periodic table of elements; All contain unpaired electronics on their outermost layer; Ground state and excited energy are more approaching, produce visible light intensive selectivity is absorbed, and its spectral absorption can suppress its ionic light transmission rate each other; When their ionic concn cooperates adjustment suitable, can complementary visible light after its curve of spectrum stack all absorb and present black.In order to obtain pure black pigment, require lightness L *It is more little good more to be worth, and color and luster a *, b *Value is all less than 5.The colorant chromaticity index of this prepared is: L *: 17.03, a *: 1.30, b *: 0.98, present good black effect.
Embodiment 1
Step 1, with Fe 2O 3, Cr 2O 3, MnCO 3, CoO, SiO 2, TiO 2, pressed powder such as MgO puts into ethanol respectively and cleans at Ultrasonic Cleaners, the ultrasonic cleaning number of times is 2 times, each scavenging period is 10min, makes its dispersion to remove surface impurity and to open big coacervate; After raw material after cleaning crossed 300 eye mesh screens respectively, place in the loft drier dry 2h under 100 ℃ of temperature.
In step 2, the raw material that in step 1, obtains, take by weighing respectively: Fe 2O 320g, Cr 2O 335g, MnCO 335g, CoO 5g, SiO 22g, TiO 22.5g, MgO 0.5g.
After step 3, the raw materials mix that step 2 is taken by weighing, add an amount of ethanol, place ball mill ball-milling processing 5h, make each component thorough mixing and make the further refinement of particle.During ball-milling processing; Institute uses ball mill to be planetary ball mill; The ball grinder that uses be corundum ceramic ball grinder, zirconia ceramics ball grinder, aluminium nitride ceramics ball grinder, nylon ball grinder or urethane ball grinder, the abrading-ball that uses be corundum ceramic abrading-ball, zirconia ceramics abrading-ball, aluminium nitride ceramics abrading-ball or agate abrading-ball.
Step 4: the material that step 3 obtains is put into loft drier, dry 3h under 100 ℃ of temperature.
Step 5: the material that step 4 is obtained places crucible, is heated to 1200 ℃ in the high temperature sintering furnace, insulation 2h.
Step 6: after using mortar to pulverize the material that obtains in the step 5, the material after pulverizing crossed 300 eye mesh screens after, add an amount of ethanol, place ball mill ball-milling processing 5h.During ball-milling processing; Institute uses ball mill to be planetary ball mill; The ball grinder that uses be corundum ceramic ball grinder, zirconia ceramics ball grinder, aluminium nitride ceramics ball grinder, nylon ball grinder or urethane ball grinder, the abrading-ball that uses be corundum ceramic abrading-ball, zirconia ceramics abrading-ball, aluminium nitride ceramics abrading-ball or agate abrading-ball.
Step 7: the material that step 6 obtains is put into loft drier, and dry 3h under 100 ℃ of temperature promptly makes the Electronic Packaging pottery with spinel structure and uses black pigment.
Embodiment 2
Step 1, with Fe 2O 3, Cr 2O 3, MnCO 3, CoO, SiO 2, TiO 2, pressed powder such as MgO puts into pure water respectively and cleans at Ultrasonic Cleaners, the ultrasonic cleaning number of times is 1 time, scavenging period is 20min, makes its dispersion to remove surface impurity and to open big coacervate; After raw material after cleaning crossed 300 eye mesh screens respectively, place in the loft drier dry 1h under 120 ℃ of temperature.
In step 2, the raw material that in step 1, obtains, take by weighing respectively: Fe 2O 330g, Cr 2O 330g, MnCO 334g, SiO 21.5g, TiO 22g, MgO 2.5g;
After step 3, the raw materials mix that step 2 is taken by weighing, add appropriate amount of purified water, place ball mill ball-milling processing 8h, make each component thorough mixing and make the further refinement of particle.During ball-milling processing; Institute uses ball mill to be planetary ball mill; The ball grinder that uses be corundum ceramic ball grinder, zirconia ceramics ball grinder, aluminium nitride ceramics ball grinder, nylon ball grinder or urethane ball grinder, the abrading-ball that uses be corundum ceramic abrading-ball, zirconia ceramics abrading-ball, aluminium nitride ceramics abrading-ball or agate abrading-ball.
Step 4: the material that step 3 obtains is put into loft drier, dry 1h under 120 ℃ of temperature.
Step 5: the material that step 4 is obtained places crucible, is heated to 1350 ℃ in the high temperature sintering furnace, insulation 1h.
Step 6: after using mortar to pulverize the material that obtains in the step 5, the material after pulverizing is crossed 300 eye mesh screens, add appropriate amount of purified water, place ball mill ball-milling processing 3h.During ball-milling processing; Institute uses ball mill to be planetary ball mill; The ball grinder that uses be corundum ceramic ball grinder, zirconia ceramics ball grinder, aluminium nitride ceramics ball grinder, nylon ball grinder or urethane ball grinder, the abrading-ball that uses be corundum ceramic abrading-ball, zirconia ceramics abrading-ball, aluminium nitride ceramics abrading-ball or agate abrading-ball.
Step 7: the material that step 6 obtains is put into loft drier, and dry 2h under 110 ℃ of temperature promptly makes the Electronic Packaging pottery with spinel structure and uses black pigment.As shown in Figure 1, be the ceramic x x ray diffration pattern x of Electronic Packaging that present embodiment makes with black pigment.As can be seen from the figure, the crystalline structure of prepared black pigment is a spinel structure, and its structural formula is (Mn, Fe) Cr 2O 4, Mn, Fe are positioned among four oxonium ions encirclements, form [AO 4] tetrahedron, Cr is positioned among six oxonium ions encirclements, forms [BO 6] octahedron.
Embodiment 3
Step 1, with Fe 2O 3, Cr 2O 3, MnCO 3, CoO, SiO 2, TiO 2, pressed powder such as MgO puts into toluene respectively and cleans at Ultrasonic Cleaners, the ultrasonic cleaning number of times is 2 times, each scavenging period is 15min, makes its dispersion to remove surface impurity and to open big coacervate; After raw material after cleaning crossed 300 eye mesh screens respectively, place in the loft drier dry 2h under 110 ℃ of temperature.
In step 2, the raw material that in step 1, obtains, take by weighing respectively: Fe 2O 327g, Cr 2O 333g, MnCO 330.5g, CoO 5g, SiO 21g, TiO 21.5g, MgO 2g;
After step 3, the raw materials mix that step 2 is taken by weighing, add an amount of toluene, place ball mill ball-milling processing 4h, make each component thorough mixing and make the further refinement of particle.During ball-milling processing; Institute uses ball mill to be planetary ball mill; The ball grinder that uses be corundum ceramic ball grinder, zirconia ceramics ball grinder, aluminium nitride ceramics ball grinder, nylon ball grinder or urethane ball grinder, the abrading-ball that uses be corundum ceramic abrading-ball, zirconia ceramics abrading-ball, aluminium nitride ceramics abrading-ball or agate abrading-ball.
Step 4: the material that step 3 obtains is put into loft drier, dry 2h under 110 ℃ of temperature;
Step 5: the material that step 4 is obtained places crucible, is heated to 1300 ℃ in the high temperature sintering furnace, insulation 1.5h;
Step 6: after using mortar to pulverize the material that obtains in the step 5, the material after pulverizing crossed 300 eye mesh screens after, add an amount of ethanol, place ball mill ball-milling processing 4h.During ball-milling processing; Institute uses ball mill to be planetary ball mill; The ball grinder that uses be corundum ceramic ball grinder, zirconia ceramics ball grinder, aluminium nitride ceramics ball grinder, nylon ball grinder or urethane ball grinder, the abrading-ball that uses be corundum ceramic abrading-ball, zirconia ceramics abrading-ball, aluminium nitride ceramics abrading-ball or agate abrading-ball.
Step 7: the material that step 6 obtains is put into loft drier, and dry 3h under 100 ℃ of temperature promptly makes the Electronic Packaging pottery with spinel structure and uses black pigment.
As shown in Figure 2, the Electronic Packaging pottery of the present invention's preparation is with the black pigment particle form is good, median size is moderate, even particle size distribution.The Electronic Packaging pottery that present embodiment is made uses the black pigment addition to be 4% of stupalith gross weight; The sintering aid addition is 6% of a stupalith gross weight; All the other are aluminum oxide, after compression moulding in the electron scanning micrograph of 1300 ℃ of agglomerating aluminum oxide packaging ceramic substrates.As can be seen from Figure 3; The alumina-ceramic of the Electronic Packaging pottery that adds this present invention after with black pigment and sintering aid; Pattern influence to alumina ceramic grain is little, and the colorant even dispersion distributes, and the part colorant is coated on the alumina particle top layer after high temperature melting.
Embodiment 4
Step 1, with Fe 2O 3, Cr 2O 3, MnCO 3, CoO, SiO 2, TiO 2, pressed powder such as MgO puts into acetone respectively and cleans at Ultrasonic Cleaners, the ultrasonic cleaning number of times is 1 time, scavenging period is 30min, makes its dispersion to remove surface impurity and to open big coacervate; After raw material after cleaning crossed 300 eye mesh screens respectively, place in the loft drier dry 2h under 100 ℃ of temperature.
In step 2, the raw material that in step 1, obtains, take by weighing respectively: Fe 2O 330g, Cr 2O 335g, MnCO 325g, CoO 4.5g, SiO 21.5g, TiO 22g, MgO 2g;
After step 3, the raw materials mix that step 2 is taken by weighing, add proper amount of acetone, place ball mill ball-milling processing 10h, make each component thorough mixing and make the further refinement of particle.During ball-milling processing; Institute uses ball mill to be planetary ball mill; The ball grinder that uses be corundum ceramic ball grinder, zirconia ceramics ball grinder, aluminium nitride ceramics ball grinder, nylon ball grinder or urethane ball grinder, the abrading-ball that uses be corundum ceramic abrading-ball, zirconia ceramics abrading-ball, aluminium nitride ceramics abrading-ball or agate abrading-ball.
Step 4: the material that step 3 obtains is put into loft drier, dry 3h under 100 ℃ of temperature;
Step 5: the material that step 4 is obtained places crucible, is heated to 1350 ℃ in the high temperature sintering furnace, insulation 1h;
Step 6: after using mortar to pulverize the material that obtains in the step 5, the material after pulverizing crossed 300 eye mesh screens after, add an amount of ethanol, place ball mill ball-milling processing 4h.During ball-milling processing; Institute uses ball mill to be planetary ball mill; The ball grinder that uses be corundum ceramic ball grinder, zirconia ceramics ball grinder, aluminium nitride ceramics ball grinder, nylon ball grinder or urethane ball grinder, the abrading-ball that uses be corundum ceramic abrading-ball, zirconia ceramics abrading-ball, aluminium nitride ceramics abrading-ball or agate abrading-ball.
Step 7: the material that step 6 obtains is put into loft drier, and dry 1h under 120 ℃ of temperature promptly makes the Electronic Packaging pottery with spinel structure and uses black pigment.

Claims (5)

1. an Electronic Packaging pottery is used black pigment, it is characterized in that, according to weight percent, is made up of following feed composition: Fe 2O 320%～30%, Cr 2O 330%～35%, MnCO 325%～35%, CoO 0%～5%, SiO 21%～2%, TiO 21.5%～2.5%, MgO 0.5%～2.5%, more than each weight percentages of components sum be 100%.
2. Electronic Packaging pottery is characterized in that with the preparation method of black pigment concrete steps are following:
Step 1, with Fe 2O 3, Cr 2O 3, MnCO 3, CoO, SiO 2, TiO 2, the MgO solid material puts into solvent respectively and cleans at Ultrasonic Cleaners, the raw material after cleaning is crossed screen cloth respectively after, place the loft drier inner drying;
In step 2, the raw material that in step 1, obtains, take by weighing respectively according to weight percent: Fe 2O 320%～30%, Cr 2O 330%～35%, MnCO 325%～35%, CoO 0%～5%, SiO 21%～2%, TiO 21.5%～2.5%, MgO 0.5%～2.5%, more than each weight percentages of components sum be 100%;
After step 3, the raw materials mix that step 2 is taken by weighing, add an amount of solvent, place ball mill ball-milling processing 4h～10h;
Step 4: the material that step 3 obtains is put into loft drier, dry 1h～3h under 100 ℃～120 ℃ temperature;
Step 5: the material that step 4 is obtained places crucible, is heated to 1200 ℃～1350 ℃ in the high temperature sintering furnace, insulation 1h～2h;
Step 6: after the material that obtains in the step 5 pulverized, cross 300 eye mesh screens, add an amount of solvent, place ball mill ball-milling processing 3h～5h;
Step 7: the material that step 6 obtains is put into loft drier, and dry 1h～3h under 100 ℃～120 ℃ temperature promptly makes.
3. according to the preparation method of the said Electronic Packaging pottery of claim 2 with black pigment, it is characterized in that in the step 1, the ultrasonic cleaning number of times is 1～2 time, each scavenging period is 10min～30min.
4. according to the preparation method of the said Electronic Packaging pottery of claim 2, it is characterized in that in step 1, step 3 and the step 6, employed solvent is pure water, ethanol, acetone or toluene with black pigment.
5. according to the preparation method of the said Electronic Packaging pottery of claim 2 with black pigment; It is characterized in that; In step 3 and the step 6, during ball-milling processing, institute uses ball mill to be planetary ball mill; The ball grinder that uses be corundum ceramic ball grinder, zirconia ceramics ball grinder, aluminium nitride ceramics ball grinder, nylon ball grinder or urethane ball grinder, the abrading-ball that uses be corundum ceramic abrading-ball, zirconia ceramics abrading-ball, aluminium nitride ceramics abrading-ball or agate abrading-ball.
CN 201110417592 2011-12-13 2011-12-13 Black pigment for electronic packaging ceramic and preparation method thereof Expired - Fee Related CN102515848B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105778566A (en) * 2016-02-29 2016-07-20 三祥新材股份有限公司 Method for preparing pigment with manganese carbonate
CN106083196A (en) * 2016-06-03 2016-11-09 深圳振华富电子有限公司 Ceramic printing slurry and its preparation method and application
CN107954698A (en) * 2017-12-20 2018-04-24 长沙市西欧电子科技有限公司 A kind of black alumina of high ceramic performance and preparation method thereof
CN112552077A (en) * 2020-12-24 2021-03-26 陕西科技大学 Black alumina ceramic and preparation method thereof
CN113651607A (en) * 2021-08-12 2021-11-16 广东宏宇新型材料有限公司 Ceramic tile with night sky and river decoration effect
CN114907705A (en) * 2022-06-22 2022-08-16 景德镇陶瓷大学 Rutile type black pigment and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
徐雷: "流延法制备黑色氧化铝陶瓷基板工艺及其性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105778566A (en) * 2016-02-29 2016-07-20 三祥新材股份有限公司 Method for preparing pigment with manganese carbonate
CN106083196A (en) * 2016-06-03 2016-11-09 深圳振华富电子有限公司 Ceramic printing slurry and its preparation method and application
CN107954698A (en) * 2017-12-20 2018-04-24 长沙市西欧电子科技有限公司 A kind of black alumina of high ceramic performance and preparation method thereof
CN112552077A (en) * 2020-12-24 2021-03-26 陕西科技大学 Black alumina ceramic and preparation method thereof
CN113651607A (en) * 2021-08-12 2021-11-16 广东宏宇新型材料有限公司 Ceramic tile with night sky and river decoration effect
CN114907705A (en) * 2022-06-22 2022-08-16 景德镇陶瓷大学 Rutile type black pigment and preparation method thereof
CN114907705B (en) * 2022-06-22 2023-06-06 景德镇陶瓷大学 Rutile type black pigment and preparation method thereof

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