CN106586983A - Preparation method of aluminum nitride powder used for heat conduction filler - Google Patents
Preparation method of aluminum nitride powder used for heat conduction filler Download PDFInfo
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- CN106586983A CN106586983A CN201610933740.XA CN201610933740A CN106586983A CN 106586983 A CN106586983 A CN 106586983A CN 201610933740 A CN201610933740 A CN 201610933740A CN 106586983 A CN106586983 A CN 106586983A
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- aluminium nitride
- nitride powder
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- heat filling
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
- C01B21/0726—Preparation by carboreductive nitridation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
- C01B21/0728—After-treatment, e.g. grinding, purification
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/40—Compounds of aluminium
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT 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
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
Abstract
The invention provides an aluminum nitride powder having high filing content and excellent hydrolysis resistance and having good compatibility with a polymeric material, and a preparation method thereof. The aluminum nitride powder can be applied to the field of fillers of heat conduction polymer materials. Carbon black and gamma-alumina which are adopted as main raw materials are nitrogenized at 1500-1800 DEG C in nitrogen atmosphere; obtained powder is decarbonized at 500-700 DEG C in specific atmosphere to obtain powder with the aluminum nitride crystal phase content of 100% and the median particle size of 5-30 [mu]m; and the obtained powder is modified with a coupling agent to obtain the aluminum nitride powder having excellent hydrolysis resistance and having good compatibility with the polymeric material. The aluminum nitride powder is suitable for the field of heat conduction plastic fillers.
Description
Technical field
The invention belongs to powder body preparation field, specially a kind of preparation method of heat filling aluminium nitride powder.
Background technology
As electronic device density increases the requirement with fast integration circuit, the radiating to microelectronic packaging material becomes to get over
Come more important.Macromolecule thermal-conducting composite material due to its high-insulativity, can fabrication design degree it is high, in radiating the advantages of corrosion-resistant
Material Field is widely used, and is a kind of Jing for solving material heat dissipation problem with high heat conduction Inorganic Fillers Filled macromolecule
Help effective method.Conventional heat filling has：Al2O3, the metal-oxide such as MgO, BeO, ZnO, AlN, BN, Si3N4Deng nitridation
Thing, and SiC, B4C3Deng carbide.Wherein, AlN is because with highly thermally conductive, excellent dielectric properties, realizing high filler loading capacity, nontoxic
The advantages of, it is particularly suitable for doing the inserts of thermal conductive insulation glue.Though aluminium nitride has many advantages, such as, the characteristics of its facile hydrolysis and
The compatibility issue of macromolecular material is also that macromolecule thermal-conducting composite material thermal conductivity of the restriction with aluminium nitride as filler is improved
Two key factors.
Aluminium nitride powder easily forms aluminium hydroxide and NH with hydroxyl in water in moist environment4 +.Aluminium nitride powder surface
The aluminum hydroxide layer of formation causes aluminium nitride lattice to dissolve in substantial amounts of oxygen, deteriorates its heat conduction and heat radiation performance；NH4 +Urging in filler
Agent has very big adverse effect.Meanwhile, aluminium nitride powder surface hydrolysiss can affect the solidification of silica gel piece, and during molding, surface has
The phenomenons such as bubble；During the use of high-power bulb, temperature is increased to more than 100 DEG C, untreated aluminium nitride powder silicon
Fat prod can be reacted with vapor, so as to affect the life-span of silicone grease.
The aluminium nitride powder of long time without surface modification and the poor compatibility of macromolecular material, i.e., it is difficult to mix with macromolecular material
Uniformly, therefore good passage of heat, an interpenetrating networks are hardly formed, it is difficult to solve high molecular conduction heat transfer.
The content of the invention
The present invention goes out from the hydrolytic Resistance for improving aluminium nitride powder and with two angles of compatibility of macromolecular material
Send out, there is provided a kind of preparation method of heat filling aluminium nitride powder.Aluminium nitride powder prepared by the method has loading
High, hydrolytic Resistance is excellent, and macromolecular material compatibility it is good the advantages of.Specifically include following steps：
Step one, dispensing：Gama-alumina is pressed into 1 with white carbon black:1.5~1:4 ratio mixing, it is extra add quality of alumina 0 ~
10% CaF2、CaO、Y2O3In one or more, and mix homogeneously.
Step 2, nitridation：Raw material is put in graphite crucible, 1 ~ 4h is nitrogenized in nitrogen atmosphere in 1500 ~ 1800 DEG C.
Step 3, except carbon：Powder body after nitridation is carried out into carbon removal treatment.Concrete operation method is to enter in air atmosphere
OK, temperature is 650 ~ 700 DEG C, except the carbon time is 1 ~ 3h；Or in the low nitrogen of hyperoxia（For relative atmospheric）Atmosphere under carry out, except carbon
Temperature is 550 ~ 650 DEG C, except the carbon time is 1 ~ 3h.
Step 4, surface treatment：Powder body is carried out using 0.5 ~ 10% coupling agent KH550, KH570, KH590, titanate esters
Surface is modified, to improve the hydrolytic Resistance and compatibility with macromolecular material of powder body.Concrete operations are as follows：By modifying agent with
After dehydrated alcohol mix homogeneously, aluminium nitride, and ball milling are added.Mill Jie ball is silicon nitride ball, zirconia ball or agate ball, after ball milling
Dry under vacuum or protective atmosphere.Ratio of grinding media to material, ball level match somebody with somebody and Ball-milling Time according to the starting particle size and demand of powder body depending on.
Modified powder body, sucking filtration, washing, drying.
Description of the drawings
Fig. 1 is the XRD spectrum of powder sample prepared by embodiment 1.
Fig. 2 is the scanning electron microscopic picture of powder sample prepared by embodiment 1.
Fig. 3 is the particle size distribution figure of powder sample prepared by embodiment 1.
Specific embodiment
The present invention is explained in detail below in conjunction with drawings and Examples.
Embodiment 1：
By 1:2.5 ratio weighs gama-alumina and white carbon black, and with quality of alumina 2%CaF2And 3% Y2O3After mix homogeneously,
It is put in graphite crucible, 2h is nitrogenized in nitrogen atmosphere in 1600 DEG C.By the sample for obtaining in 650 DEG C of the low blanket of nitrogen of hyperoxia
（Oxygen nitrogen volume ratio is 6:4）In remove carbon 1h.Jing tests obtain the sample that aluminium nitride crystalline phase is that 100%, D50 is 9.09 μm.By sample
Product：Agate ball：Dehydrated alcohol=100x:200x:The proportioning of 100x is weighed, and charging sequence is that 1x g titanate esters are anhydrous with 100x mL
After ethanol mix homogeneously, the silicon nitride ball for adding 100x g aluminium nitride powders and 100x g to match somebody with somebody without size class, rotational speed of ball-mill is
200r/min, obtains the powder body that D50 is 8 μm after ball milling 2h.Modified powder body, sucking filtration, washing, drying.Take sample 1g to exist
In floating shape, to settle without granule after 24h in 50 DEG C of water, activation index is 1 to 50mL temperature.
To illustrate the excellent properties of nitridation Al filler that this patent prepares, the sample that embodiment 1 is prepared is used for low temperature
The liquid silastic filler of sulfuration, and test its thermal conductivity.Base material is made from low viscous vinyl silicone oil, hydrogen content is relatively low
Containing hydrogen silicone oil is cross-linking agent.Karstedt catalyst:The mass fraction of platinum is 1.0 × 10-4；Acetylene Hexalin inhibitor:Suppress
Agent（mol）/Pt（mol）=1600.After 9g base materials, 20g cross-linking agent, 2g catalyst, 2g inhibitor are mixed homogeneously with 180g fillers
It is put in mould, and the evacuation in vacuum pump.120 DEG C are heated in being then placed in stove, and are incubated 30min to complete solidification.
Laser heat conducting instrument is adopted to test its thermal conductivity after the demoulding for 1.92 W/ (mK).
Embodiment 2：
By 1:1.5 ratio weighs gama-alumina and white carbon black, and after mixing homogeneously with the CaO of quality of alumina 10%, is put into stone
In black crucible, 4h is nitrogenized in nitrogen atmosphere in 1500 DEG C.By the sample for obtaining in 650 DEG C of air atmosphere remove carbon 3h.Jing
Test obtains the sample that aluminium nitride crystalline phase is that 100%, D50 is 5.15 μm.Because of granularity and general filler powder body minimum particle size phase
When, therefore powder body does not need further micronization processes.The powder body 100g for weighing above-mentioned preparation adds 0.5gKH570 and 100mL's
In the mixed solution of dehydrated alcohol, stir, and ball milling.Using silicon nitride mill Jie's ball of diameter 5mm, ratio of grinding media to material is 3:2, turn
Fast 200r/min, ball milling 2h.Modified powder body, sucking filtration, drying.Obtain hydrolytic Resistance excellent, compatible with macromolecular material
The good aluminium nitride powder of property.
Embodiment 3：
Gama-alumina is pressed into 1 with white carbon black:It is put in graphite crucible after 4 ratio mix homogeneously, in 1800 DEG C in nitrogen atmosphere
Nitridation 1h.By the sample for obtaining in 700 DEG C of air atmosphere remove carbon 1h.Jing tests obtain aluminium nitride crystalline phase and for 100%, D50 are
29.57 μm sample.By sample：Zirconia ball：Dehydrated alcohol=100x:300x:The proportioning of 100x is weighed, and charging sequence is
After 10x gKH550 are mixed homogeneously with 100x mL dehydrated alcohol, 100x g aluminium nitride powders and 300x g is added to have size class to match somebody with somebody
Zirconia ball, rotational speed of ball-mill is 500r/min, and the powder body that D50 is 12 μm is obtained after ball milling 2h.Modified powder body, sucking filtration,
Drying.Obtain that hydrolytic Resistance is excellent, and the macromolecular material good aluminium nitride powder of compatibility.
Embodiment 4：
By 1:3 ratio weighs gama-alumina and white carbon black, and the Y with quality of alumina 5%2O3After mix homogeneously, graphite is put into
In crucible, 2h is nitrogenized in nitrogen atmosphere in 1700 DEG C.By the sample for obtaining in 550 DEG C of the low blanket of nitrogen of hyperoxia（Oxygen nitrogen volume
Than for 5:5）In remove carbon 3h.Jing tests obtain the sample that aluminium nitride crystalline phase is that 100%, D50 is 19.96 μm.By sample：Achatess
Ball：Dehydrated alcohol=100x:200x:The proportioning of 100x is weighed, and charging sequence is mixed with 100x mL dehydrated alcohol for 5x gKH590
After uniform, 100x g aluminium nitride powders and 200x g is added to have a zirconia ball that size class is matched somebody with somebody, rotational speed of ball-mill is 300r/min, ball
The powder body that D50 is 10 μm is obtained after mill 2h.Modified powder body, sucking filtration, drying.Obtain that hydrolytic Resistance is excellent, and macromolecule
The good aluminium nitride powder of material compatibility.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more concrete and detailed, but can not
Therefore it is interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art,
Without departing from the inventive concept of the premise, some deformations and improvement can also be made, these belong to the protection model of the present invention
Enclose.Therefore, the protection domain of patent of the present invention should be defined by claims.
Claims (8)
1. a kind of preparation method of heat filling aluminium nitride powder, including dispensing, nitridation, except carbon, surface treatment 4 is main walks
Suddenly, the sample prepared is that loading is high, hydrolytic Resistance is excellent, and the good aluminium nitride powder of macromolecular material compatibility, its
It is characterised by：
Step one, dispensing：Gama-alumina is mixed by a certain percentage with white carbon black, a certain amount of additive is additionally added, and is mixed
Uniformly；
Step 2, nitridation：Raw material is put in graphite crucible, is nitrogenized in nitrogen atmosphere under high temperature；
Step 3, except carbon：Powder body after nitridation is carried out into carbon removal treatment；
The optimization of step 4, surface treatment and granularity：Table is carried out by way of ball milling coupling agent, dehydrated alcohol and aluminium nitride sample
Face is modified, to improve the hydrolytic Resistance and compatibility with macromolecular material of powder body；If it is desired, this step can be by adjusting ball
Material ratio, mill Jie's ball level are matched somebody with somebody and Ball-milling Time and rotating speed, and powder granularity is optimized.
2. a kind of preparation method of heat filling aluminium nitride powder according to claim 1, is characterized in that：Described step
In rapid one, the ratio of gama-alumina and white carbon black is 1:1.5~1:4.
3. a kind of preparation method of heat filling aluminium nitride powder according to claim 1, is characterized in that：Described step
In rapid one, additive is CaF2、CaO、Y2O3In one or more；Addition for quality of alumina 0 ~ 10%.
4. a kind of preparation method of heat filling aluminium nitride powder according to claim 1, is characterized in that：Described step
In rapid two, nitriding temperature is 1500 ~ 1800 DEG C, and nitridation time is 1 ~ 4h.
5. a kind of preparation method of heat filling aluminium nitride powder according to claim 1, is characterized in that：Described step
In rapid three, except carbon is carried out in air atmosphere, temperature is 650 ~ 700 DEG C, except the carbon time is 1 ~ 3h；Or in the low nitrogen of hyperoxia（Relatively
For air）Atmosphere under carry out, except carbon temperature be 550 ~ 650 DEG C, except the carbon time be 1 ~ 3h.
6. a kind of preparation method of heat filling aluminium nitride powder according to claim 1, is characterized in that：Described step
In rapid four, the coupling agent that is modified is KH550, KH570, KH590, titanate esters, and addition is 0.5 ~ 10%；Modified flow process is aluminium nitride
After mixing with dehydrated alcohol, modifying agent, and ball milling are added；Modified powder body, sucking filtration, washing, drying.
7. a kind of preparation method of heat filling aluminium nitride powder according to claim 1, is characterized in that：Prepare
Sample is that loading is high, hydrolytic Resistance is excellent, and the good aluminium nitride powder of macromolecular material compatibility.
8. a kind of preparation method of heat filling aluminium nitride powder according to claim 1, is characterized in that：It is applied to lead
Hot filler field.
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| CN201610933740.XA CN106586983A (en) | 2016-11-01 | 2016-11-01 | Preparation method of aluminum nitride powder used for heat conduction filler |
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| CN201610933740.XA CN106586983A (en) | 2016-11-01 | 2016-11-01 | Preparation method of aluminum nitride powder used for heat conduction filler |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106699189A (en) * | 2016-11-25 | 2017-05-24 | 河北利福光电技术有限公司 | Aluminum nitride powder for aluminum nitride ceramic substrate and preparation method of aluminum nitride powder |
| CN107954725A (en) * | 2017-11-29 | 2018-04-24 | 上海宇昂水性新材料科技股份有限公司 | Resistant to hydrolysis aluminium nitride powder and preparation method thereof |
| CN108949114A (en) * | 2018-07-23 | 2018-12-07 | 湖南宁乡吉唯信金属粉体有限公司 | A kind of powder stuffing preparation method for heat conductive insulating interface |
| CN114031409A (en) * | 2021-11-29 | 2022-02-11 | 航天特种材料及工艺技术研究所 | Preparation method of high-purity aluminum nitride powder for high-thermal-conductivity filler |
| CN114031050A (en) * | 2021-11-29 | 2022-02-11 | 航天特种材料及工艺技术研究所 | Preparation method of high-purity aluminum nitride powder |
-
2016
- 2016-11-01 CN CN201610933740.XA patent/CN106586983A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106699189A (en) * | 2016-11-25 | 2017-05-24 | 河北利福光电技术有限公司 | Aluminum nitride powder for aluminum nitride ceramic substrate and preparation method of aluminum nitride powder |
| CN107954725A (en) * | 2017-11-29 | 2018-04-24 | 上海宇昂水性新材料科技股份有限公司 | Resistant to hydrolysis aluminium nitride powder and preparation method thereof |
| CN108949114A (en) * | 2018-07-23 | 2018-12-07 | 湖南宁乡吉唯信金属粉体有限公司 | A kind of powder stuffing preparation method for heat conductive insulating interface |
| CN114031409A (en) * | 2021-11-29 | 2022-02-11 | 航天特种材料及工艺技术研究所 | Preparation method of high-purity aluminum nitride powder for high-thermal-conductivity filler |
| CN114031050A (en) * | 2021-11-29 | 2022-02-11 | 航天特种材料及工艺技术研究所 | Preparation method of high-purity aluminum nitride powder |
| CN114031409B (en) * | 2021-11-29 | 2022-09-23 | 航天特种材料及工艺技术研究所 | Preparation method of high-purity aluminum nitride powder for high-thermal-conductivity filler |
| CN114031050B (en) * | 2021-11-29 | 2022-11-15 | 航天特种材料及工艺技术研究所 | Preparation method of high-purity aluminum nitride powder |
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Application publication date: 20170426 |