CN108689716A - The preparation method of high thermal-conductivity aluminum nitride ceramics structural member - Google Patents
The preparation method of high thermal-conductivity aluminum nitride ceramics structural member Download PDFInfo
- Publication number
- CN108689716A CN108689716A CN201810368415.2A CN201810368415A CN108689716A CN 108689716 A CN108689716 A CN 108689716A CN 201810368415 A CN201810368415 A CN 201810368415A CN 108689716 A CN108689716 A CN 108689716A
- Authority
- CN
- China
- Prior art keywords
- temperature
- structural member
- high thermal
- powder
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C04B35/581—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 aluminium nitride
-
- 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/6267—Pyrolysis, carbonisation or auto-combustion reactions
-
- 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/6342—Polyvinylacetals, e.g. polyvinylbutyral [PVB]
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient
Abstract
A kind of preparation method of high thermal-conductivity aluminum nitride ceramics structural member, this method by aluminium nitride powder, organic solvent, dispersant, binder carry out mixed grinding, be then spray-dried, sieved successively, being suppressed, dumping, sintering;The beneficial effects of the present invention are:Using effective control to oxygen in the aluminium nitride powder of low oxygen content and slurrying, dumping, sintering process, it ensure that the aluminium nitride ceramics structural member of preparation has high thermal conductivity;It is matched using the powder of moderate dispersant, binder, so that the first spherical mixed powder is prepared in spray drying, and rational second temperature system when further by controlling the second mixed powder size distribution and when dumping rational first temperature schedule, sintering, it ensure that the aluminium nitride ceramics of preparation has high thermal conductivity and high consistency;In addition, rational first temperature schedule, second temperature institutional guarantee green body are indeformable in dumping and sintering, the surfacing of aluminium nitride ceramics structural member ensure that.
Description
Technical field
The present invention relates to advanced ceramics molding and processing technique field, more particularly to a kind of high thermal-conductivity aluminum nitride ceramics structures
The preparation method of part.
Background technology
Compared with traditional ceramics material, the advanced ceramics material with good characteristic and function is widely used in national warp
The every field of Ji, multiple countries of the world put into the research that a large amount of manpower and financial resources carries out new ceramic material.Aluminium oxide, oxygen
Change beryllium, silicon carbide ceramics with excellent characteristic and stability, is current application ceramic material the most ripe, most common.Nitrogen
Changing aluminium ceramics has low high heat conductance, low-k, low linear expansion coefficient, density, nontoxic, high mechanical strength and insulation performance
Well equal good characteristics, are widely used in high-power integrated circuit, modular circuit, microelectronics, optics, communication, electrical part and intelligence
The fields such as energy manufacture.In view of its excellent performance and extensive use, by as 21 century is highly thermally conductive, high intensity, the master in terms of insulation
New material is flowed, foreground is had a vast market, causes the extensive concern of people.The study found that the theoretical thermal conductivity of aluminium nitride is
320W/ (mk), but because preparing aerobic in aluminium nitride ceramics lattice and impurity incorporation, make the reduction of its thermal conductivity, and prepare
Aluminium nitride ceramics consistency it is not high, it is yielding, make its surface irregularity, these all affect the popularization and application of aluminium nitride ceramics
Invention content
In view of this, against the above deficiency, it is necessary to propose that a kind of aluminium nitride ceramics structural member thermal conductivity prepared is high, cause
Density is high, is unlikely to deform, the preparation method of the high thermal-conductivity aluminum nitride ceramics structural member of surfacing.
A kind of preparation method of high thermal-conductivity aluminum nitride ceramics structural member, this approach includes the following steps:
Step 1:Aluminium nitride powder is added to the first organic solvent, and carries out mixed grinding, obtains the first mixed slurry,
In, the quality of the first organic solvent:The quality of aluminium nitride powder=(2~3):(2~3), the average grain of the aluminium nitride powder
Diameter D50 is 1.0~3.0um, and the oxygen content of the aluminium nitride powder is 1.0~1.5wt%;
Step 2:Sintering aid, dispersant are added the first mixed slurry, and mixed grinding by a certain percentage successively, obtain the
Two mixed slurries;
Step 3:By binder with the second organic solvent heat of solution it is uniform after, by the mixture of binder and the second organic solvent
The second mixed slurry, and mixed grinding is added, obtains third mixed slurry;
Step 4:The third mixed slurry is spray-dried, to obtain spherical first mixed powder;
Step 5:First mixed powder is sieved using the mesh screen of 80 mesh or 100 mesh, takes the screenings conduct of mixed powder
Second mixed powder;
Step 6:Second mixed powder is pressed into green body, typed pressure is controlled in 50~150MPa;
Step 7:The green body is packed into atmosphere furnace, and carries out dumping under the first temperature schedule, is passed through in the atmosphere furnace
Compressed air or by the atmosphere stove evacuation, first temperature schedule is that heating rate is controlled in 0.2~0.5 DEG C/min,
Intermediate stage multistage is kept the temperature, and the control of high temperature section temperature is at 400~600 DEG C and keeps the temperature 5~6 hours;
Step 8:Green body after dumping is packed into sintering furnace, and is sintered under second temperature system, to obtain high thermal-conductivity aluminum nitride
Ceramic structures, the second temperature system are:When heating, heating rate is 5~10 DEG C/min before 1000 DEG C, 1550
Heating rate is 3~6 DEG C/min, 0.1~3 DEG C/min of heating rate before 1850 DEG C, 1760~1850 DEG C of heat preservations 1 before DEG C
~10 hours, intermediate stage multistage kept the temperature 0.5~2 hour, and when cooling, 1000 DEG C are down to the rate of temperature fall of 2~10 DEG C/min,
Room temperature is down to the rate of temperature fall of 5~20 DEG C/min again, the sintering furnace is high pure nitrogen atmosphere.
The beneficial effects of the present invention are:Using the aluminium nitride powder of low oxygen content and slurrying, dumping, sintering process
In effective control to oxygen, effectively avoid the incorporation for preparing oxygen in aluminium nitride ceramics structural member lattice, ensure that preparation
Aluminium nitride ceramics structural member has high thermal conductivity;It is matched using the powder of moderate dispersant, binder, so that spray drying
Prepare the first mixed powder of even-grained superfine spherical, and further by control the second mixed powder size distribution with
And rational second temperature system when rational first temperature schedule when dumping, sintering, it ensure that the aluminium nitride ceramics knot of preparation
Component has high thermal conductivity and high consistency;In addition, rational first temperature schedule, second temperature institutional guarantee green body
It is indeformable in dumping and sintering, it ensure that the surfacing of aluminium nitride ceramics structural member.
Description of the drawings
Fig. 1 is the process flow chart of the preparation method of high thermal-conductivity aluminum nitride ceramics structural member.
Specific implementation mode
In order to illustrate the technical solution of the embodiments of the present invention more clearly, being carried out further below in conjunction with embodiment
It is bright.
The present invention provides a kind of preparation methods of high thermal-conductivity aluminum nitride ceramics structural member, and this approach includes the following steps:
S301:Aluminium nitride powder is added to the first organic solvent, and carries out mixed grinding, obtains the first mixed slurry, wherein
The quality of first organic solvent:The quality of aluminium nitride powder=(2~3):The average grain diameter D50 of (2~3), aluminium nitride powder is
The oxygen content of 1.0~3.0um, aluminium nitride powder are 1.0~1.5wt%;
For example, using Ball-stirring mill mixed grinding, first the first organic solvent is added to Ball-stirring mill, then starts Ball-stirring mill, then add
Enter aluminium nitride powder, then proceedes to mixed grinding.
It is preferred that using the aluminium nitride powder prepared by carbothermic method or self- propagating method, aluminium nitride meets water capacity facile hydrolysis, and
If adopting water as solvent, the oxygen contained in water can influence the thermal conductivity of end article;First organic solvent is preferably anhydrous second
Alcohol, the quality of preferred first organic solvent:Quality=1 of aluminium nitride powder:1.
S302:The first mixed slurry, and mixed grinding is added in sintering aid, dispersant by a certain percentage successively, is obtained
Second mixed slurry;
Sintering aid is the first sintering aid or the second sintering aid, and the first sintering aid is preferably the oxide of alkaline earth, rare earth
Oxide, the fluoride of alkaline earth, one kind in the fluoride of rare earth, the binder is polyvinyl butyral, referred to as
PVB, in terms of the quality of the aluminium nitride powder, the additive amount of the first sintering aid is 2~8wt%, and the additive amount of dispersant is 1
The additive amount of~3wt%, binder are 2~10wt%.
Second sintering aid is the complex sintering aids that yttrium oxide and calcium oxide form, and is helped for example, by using Y-Ca is complex sintered
Agent, wherein the mass percent of yttrium oxide and calcium oxide is about 1 in Y-Ca complex sintering aids:1, yttria levels are slightly on the high side.
S303:By binder with the second organic solvent heat of solution it is uniform after, by the mixing of binder and the second organic solvent
The second mixed slurry, and mixed grinding is added in object, obtains third mixed slurry;
Specifically, binder and the absolute ethyl alcohol and stirring through heating water bath is uniform, be added after it is completely dissolved Ball-stirring mill into
Row stir mixing is ground.
Second organic solvent is preferably absolute ethyl alcohol;Binder is generally difficult to be dissolved in the relatively low absolute ethyl alcohol of temperature, not
The short grained binder of dissolving can influence subsequent mist projection granulating, also be unfavorable for subsequent sintering, to influence aluminium nitride pottery
The consistency of porcelain structural member.
S304:Third mixed slurry is spray-dried, to obtain spherical first mixed powder;Spray drying can change
The physical property of aluminium nitride powder is conducive to subsequent compacting, dumping, sintering process, for example, the first mixed powder that spray drying obtains
Material, granularity is small, and particle is uniform-spherical, can greatly improve subsequent pressed density, improves consistency;Obtained green body tissue is equal
Even, when dumping is not in that local dumping amount is big, causes the deformation of idiosome;In addition, when spray drying, third mixed slurry is divided
It dissipates and greatly reduces the organic solvent in the first mixed powder after drying since drop specific surface area is very big for fine droplets, from
And reduce the generation of the volatile matter of follow-up dumping process, reduce the deformation of follow-up green body;The first mixing after spray drying
Powder, binder, sintering aid distribute very evenly, and are conducive to improve consistency when follow-up compacting.
S305:First mixed powder is sieved using the mesh screen of 80 mesh or 100 mesh, takes the screenings of mixed powder as the
Two mixed powders;So that the grain size of second mixed powder is less than 180 μm;
By the first mixed powder, it is preferable to use 80 mesh mesh screens to sieve, and the second mixed powder of spherical shape of moderate granularity can increase starting heap
Poly- density reduces powder particles gap and air content, avoids forming arch-shaped space in pressing process and increasing porosity, from
And suppress fine and close green body.
S306:Second mixed powder is pressed into green body, typed pressure is controlled in 50~150MPa;Press device is preferably
Isostatic pressing machine;Wherein, dry press can be used in small dimension blank forming, and big specification blank forming molding can be used dry press or wait quiet
Pressure;Using the continuous compression moulding of high-volume when compacting, production efficiency is high, reduces production cost, and the waste material of generation can be returned further
It receives and uses, improve powder utilization rate.
S307:Green body is packed into atmosphere furnace, and carries out dumping under the first temperature schedule, it is empty that compression is passed through in atmosphere furnace
Gas or by atmosphere stove evacuation, the first temperature schedule is that heating rate is controlled in 0.2~0.5 DEG C/min, and intermediate stage multistage is protected
Temperature, the control of high temperature section temperature is at 400~600 DEG C and keeps the temperature 5~6 hours;Wherein, when big specification thick stock body dumping shove charge reduce with
The contact area of BN loading plates keeps green body dumping more thorough;
Atmosphere furnace in temperature-rise period, between room temperature to maximum temperature within the temperature range of multiple soaking zones are set, with not
Volatile matter in green body is discharged same temperature section, prevents blank deformation, cracks;Preferred holding temperature is 80 DEG C, 200 DEG C,
310 DEG C, 450 DEG C, moderate temperature rise speed and soaking time substantially reduce the cracking of green body, deformation.
S308:Green body after dumping is packed into sintering furnace, and is sintered under second temperature system, to obtain highly thermally conductive nitridation
Aluminium ceramic structures, second temperature system are:When heating, heating rate is 5~10 DEG C/min before 1000 DEG C, at 1550 DEG C
In the past heating rate be 3~6 DEG C/min, 0.1~3 DEG C/min of heating rate 1850 DEG C before, 1760~1850 DEG C keep the temperature 1~
10 hours, intermediate stage multistage kept the temperature 0.5~2 hour, and when cooling, 1000 DEG C are down to the rate of temperature fall of 2~10 DEG C/min, then
It is down to room temperature with the rate of temperature fall of 5~20 DEG C/min, sintering furnace is high pure nitrogen atmosphere, and the pressure of nitrogen is 110KPa;Wherein,
Enough BN interlayer powder is applied when shove charge between big specification thick stock body and BN loading plates and increases lubrication, big specification is rodlike, tubulose and different
Type part shove charge uses suspending way, to reduce sintering shrinkage frictional resistance.
Aluminium nitride ceramics will generate a certain amount of contraction in high temperature sintering, and to reach densification, sintering process is different
Heating rate, sintering temperature and soaking time are affected to aluminium nitride ceramics performance, the thermal conductivity of aluminium nitride ceramics and sintering
Density can be continuously increased with the raising of sintering temperature.
In second temperature system, rational heating rate, multistage heat preservation, cooling rate can effectively eliminate furnace temperature unevenness,
Ensure that green body heat transfer is uniform, reduces the deformation of aluminium nitride ceramics structural member, and improve the consistency of aluminium nitride ceramics structural member.
Further, spray-drying process carries out under nitrogen protection atmosphere, to reduce the oxygen content of the first mixed powder,
The incorporation for avoiding oxygen in aluminium nitride ceramics structural member lattice ensure that the aluminium nitride ceramics structural member of preparation has high thermal conductivity
Rate.
Further, this method further includes the steps that pre- dumping is carried out between S305 and S306, and second in S305 is mixed
It closes powder to be packed into atmosphere furnace, compressed air is passed through in atmosphere furnace or by atmosphere stove evacuation, and carried out under the first temperature schedule
Dumping, and then dumping amount in follow-up S307 is reduced, it deforms, cracks when reducing green body dumping.
Further, in S308, before sintering furnace heating, sintering furnace stove is evacuated to 2.5 × 101Pa, in backfill High Purity Nitrogen
Gas is to 110KPa, to reduce the oxygen content in sintering atmosphere, and then meets sintering and requires;It is by purge drying to be passed through nitrogen
Liquid nitrogen, the flow for being passed through nitrogen are 0.5~5m3/h。
Further, this method further includes that will obtain high thermal-conductivity aluminum nitride ceramics structural member in S308 to carry out cold grinding polishing treatment
The step of, reach required dimensional tolerance range.
The beneficial effects of the present invention are:Using the aluminium nitride powder of low oxygen content and slurrying, dumping, sintering process
In effective control to oxygen, effectively avoid the incorporation for preparing oxygen in aluminium nitride ceramics structural member lattice, ensure that preparation
Aluminium nitride ceramics structural member has high thermal conductivity;It is matched using the powder of moderate dispersant, binder, so that spray drying
Prepare the first mixed powder of even-grained superfine spherical, and further by control the second mixed powder size distribution with
And rational second temperature system when rational first temperature schedule when dumping, sintering, it ensure that the aluminium nitride ceramics knot of preparation
Component has high thermal conductivity and high consistency;In addition, rational first temperature schedule, second temperature institutional guarantee green body
It is indeformable in dumping and sintering, it ensure that the surfacing of aluminium nitride ceramics structural member.
Below in conjunction with specific implementation mode, the present invention will be described in detail, so that those skilled in the art can be better
Understand advantages of the present invention.
Embodiment 1
Ball-stirring mill is added in absolute ethyl alcohol, starts Ball-stirring mill, by aluminium nitride powder:Absolute ethyl alcohol=1:Nitridation is added in 1 ratio
Aluminium powder material carries out mixed grinding, and the average grain diameter D50 of aluminium nitride powder is 1.0~3.0um, and the oxygen content of aluminium nitride powder is
1.0~1.5wt% adds the Y of 5wt% in terms of the quality of aluminium nitride powder2O3, 4wt%PVB, 2wt% dispersant mixed
Close grinding;It is to be mixed uniformly after be spray-dried, be used in combination 80 mesh screens sieving;Powder after sieving is using dry press compacting
Small dimension disc-shaped green body, typed pressure are controlled in 70MPa,;Green body is packed into atmosphere furnace, is heated up with the speed of 0.4 DEG C/min
To 550 DEG C and 5 hours are kept the temperature, intermediate stage holding temperature is respectively 80 DEG C, 200 DEG C, 310 DEG C, 450 DEG C;By the base after dumping
The sintering furnace that body is packed into through-flow dynamic high pure nitrogen is sintered, sintering heating when, 1000 DEG C before heating rate for 10 DEG C/
Min, before 1550 DEG C heating rate be 5 DEG C/min, 1700 DEG C before with the rate of 3 DEG C/min heating, 1780 DEG C with
The preceding rate with 1 DEG C/min heats up and keeps the temperature 1 hour, intermediate stage segmentation heat preservation 1 hour, the property of obtained aluminium nitride ceramics part
Energy index is as shown in the table.
| Project | Performance indicator |
| Density (g/cm3) | 3.32 |
| Thermal conductivity (W/mk) | 175 |
| Bending strength (Mpa) | 362 |
Embodiment 2
Ball-stirring mill is added in absolute ethyl alcohol, starts Ball-stirring mill, by aluminium nitride powder:Absolute ethyl alcohol=1:Nitridation is added in 1 ratio
Aluminium powder material carries out mixed grinding, and the average grain diameter D50 of aluminium nitride powder is 1.0~3.0um, and the oxygen content of aluminium nitride powder is
1.0~1.5wt% adds the Y of 5wt% in terms of the quality of aluminium nitride powder2O3, 8wt%PVB, 2wt% dispersant mixed
Close grinding;It is to be mixed uniformly after be spray-dried, be used in combination 80 mesh screens sieving;Powder after sieving uses dry type isostatic pressed pressure
The rodlike green body of rounding, typed pressure are controlled in 70MPa,;Green body is packed into atmosphere furnace, 600 are warming up to the speed of 0.4 DEG C/min
DEG C and keep the temperature 6 hours, intermediate stage holding temperature is respectively 80 DEG C, 200 DEG C, 310 DEG C, 450 DEG C;Green body after dumping is packed into
The sintering furnace of through-flow dynamic high pure nitrogen is sintered, and when sintering heats up, heating rate is 10 DEG C/min before 1000 DEG C,
Heating rate is 5 DEG C/min before 1550 DEG C, is heated up with the rate of 3 DEG C/min before 1700 DEG C, with 0.5 before 1800 DEG C
DEG C/rate of min heats up and keeps the temperature 5 hours, intermediate stage segmentation heat preservation 1 hour, green body uses suspending way in sintering shove charge,
The performance indicator of obtained aluminium nitride ceramics part is as shown in the table.
| Project | Performance indicator |
| Density (g/cm3) | 3.33 |
| Thermal conductivity (W/mk) | 172 |
| Bending strength (Mpa) | 385 |
Embodiment 3
Ball-stirring mill is added in absolute ethyl alcohol, starts Ball-stirring mill, by aluminium nitride powder:Absolute ethyl alcohol=1:Nitridation is added in 1 ratio
Aluminium powder material carries out mixed grinding, and the average grain diameter D50 of aluminium nitride powder is 1.0~3.0um, and the oxygen content of aluminium nitride powder is
1.0~1.5wt% adds the Y of 5wt% in terms of the quality of aluminium nitride powder2O3, 8wt%PVB, 2wt% dispersant mixed
Close grinding;It is to be mixed uniformly after be spray-dried, be used in combination 80 mesh screens sieving;Powder after sieving using powder dry press and
Isostatic pressing machine is combined the big rectangular green body of specification of compacting, and typed pressure is controlled in 70MPa,;Green body is packed into atmosphere furnace, with 0.2
DEG C/speed of min is warming up to 600 DEG C and keeps the temperature 6 hours, intermediate stage holding temperature is respectively 80 DEG C, 200 DEG C, 310 DEG C, 450
℃;Wherein, when dumping, to reduce the contact area of green body and BN loading plates, the green body after dumping is packed into through-flow dynamic High Purity Nitrogen
The sintering furnace of gas is sintered, and when sintering heats up, heating rate is 10 DEG C/min before 1000 DEG C, is heated up before 1550 DEG C
Rate is 5 DEG C/min, is heated up with the rate of 3 DEG C/min before 1700 DEG C, with the rate liter of 0.2 DEG C/min before 1820 DEG C
Temperature simultaneously keeps the temperature 8 hours, intermediate stage segmentation heat preservation 1 hour, wherein when sintering, to reduce the contact surface of green body and BN loading plates
Product, and enough BN interlayer powder are applied, to ensure that dumping is thorough and reduce sintering shrinkage frictional resistance, obtained aluminium nitride ceramics part
Performance indicator it is as shown in the table.
| Project | Performance indicator |
| Density (g/cm3) | 3.34 |
| Thermal conductivity (W/mk) | 178 |
| Bending strength (Mpa) | 406 |
The steps in the embodiment of the present invention can be sequentially adjusted, merged and deleted according to actual needs.
The above disclosure is only the preferred embodiments of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, those skilled in the art can understand all or part of the processes for realizing the above embodiment, and is wanted according to right of the present invention
Equivalent variations made by asking, still belong to the scope covered by the invention.
Claims (10)
1. a kind of preparation method of high thermal-conductivity aluminum nitride ceramics structural member, it is characterised in that:This approach includes the following steps:
Step 1:Aluminium nitride powder is added to the first organic solvent, and carries out mixed grinding, obtains the first mixed slurry,
In, the quality of the first organic solvent:The quality of aluminium nitride powder=(2~3):(2~3), the average grain diameter of the aluminium nitride powder
D50 is 1.0~3.0um, and the oxygen content of the aluminium nitride powder is 1.0~1.5wt%;
Step 2:Sintering aid, dispersant are added the first mixed slurry, and mixed grinding by a certain percentage successively, obtain the
Two mixed slurries;
Step 3:By binder with the second organic solvent heat of solution it is uniform after, by the mixture of binder and the second organic solvent
The second mixed slurry, and mixed grinding is added, obtains third mixed slurry;
Step 4:The third mixed slurry is spray-dried, to obtain spherical first mixed powder;
Step 5:First mixed powder is sieved using the mesh screen of 80 mesh or 100 mesh, takes the screenings conduct of mixed powder
Second mixed powder;
Step 6:Second mixed powder is pressed into green body, typed pressure is controlled in 50~150MPa;
Step 7:The green body is packed into atmosphere furnace, and carries out dumping under the first temperature schedule, is passed through in the atmosphere furnace
Compressed air or by the atmosphere stove evacuation, first temperature schedule is that heating rate is controlled in 0.2~0.5 DEG C/min,
Intermediate stage multistage is kept the temperature, and the control of high temperature section temperature is at 400~600 DEG C and keeps the temperature 5~6 hours;
Step 8:Green body after dumping is packed into sintering furnace, and is sintered under second temperature system, to obtain high thermal-conductivity aluminum nitride
Ceramic structures, the second temperature system are:When heating, heating rate is 5~10 DEG C/min before 1000 DEG C, 1550
Heating rate is 3~6 DEG C/min, 0.1~3 DEG C/min of heating rate before 1850 DEG C, 1760~1850 DEG C of heat preservations 1 before DEG C
~10 hours, intermediate stage multistage kept the temperature 0.5~2 hour, and when cooling, 1000 DEG C are down to the rate of temperature fall of 2~10 DEG C/min,
Room temperature is down to the rate of temperature fall of 5~20 DEG C/min again, the sintering furnace is high pure nitrogen atmosphere.
2. the preparation method of high thermal-conductivity aluminum nitride ceramics structural member as described in claim 1, it is characterised in that:Described first has
The quality of solvent:Quality=1 of aluminium nitride powder:1.
3. the preparation method of high thermal-conductivity aluminum nitride ceramics structural member as claimed in claim 2, it is characterised in that:Described first has
Solvent, the second organic solvent are absolute ethyl alcohol.
4. the preparation method of high thermal-conductivity aluminum nitride ceramics structural member as described in claim 1, it is characterised in that:The aluminium nitride
Powder prepares gained by carbothermic method or self- propagating method.
5. the preparation method of high thermal-conductivity aluminum nitride ceramics structural member as described in claim 1, it is characterised in that:The sintering helps
Agent is the first sintering aid or the second sintering aid, and first sintering aid is the oxide of alkaline earth, the oxide of rare earth, alkali
One kind in the fluoride of soil, the fluoride of rare earth, the binder is PVB, in terms of the quality of the aluminium nitride powder, first
The additive amount of sintering aid is 2~8wt%, and the additive amount of dispersant is 1~3wt%, and the additive amount of binder is 2~10wt%.
6. the preparation method of high thermal-conductivity aluminum nitride ceramics structural member as described in claim 1, it is characterised in that:Described second burns
It is the complex sintering aids that yttrium oxide and calcium oxide form to tie auxiliary agent.
7. the preparation method of high thermal-conductivity aluminum nitride ceramics structural member as described in claim 1, it is characterised in that:By described first
Mixed powder is sieved using 80 mesh mesh screens.
8. the preparation method of high thermal-conductivity aluminum nitride ceramics structural member as described in claim 1, it is characterised in that:In step 7
Holding temperature is respectively 80 DEG C, 200 DEG C, 310 DEG C, 450 DEG C.
9. the preparation method of high thermal-conductivity aluminum nitride ceramics structural member as described in claim 1, it is characterised in that:In step 8
In, before sintering furnace heating, sintering furnace stove is evacuated to 2.5 × 101Pa, in backfill high pure nitrogen to 110KPa.
10. the preparation method of high thermal-conductivity aluminum nitride ceramics structural member as described in claim 1, it is characterised in that:This method is also
Include the steps that will obtain high thermal-conductivity aluminum nitride ceramics structural member in step 8 to carry out cold grinding polishing treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810368415.2A CN108689716A (en) | 2018-04-23 | 2018-04-23 | The preparation method of high thermal-conductivity aluminum nitride ceramics structural member |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810368415.2A CN108689716A (en) | 2018-04-23 | 2018-04-23 | The preparation method of high thermal-conductivity aluminum nitride ceramics structural member |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108689716A true CN108689716A (en) | 2018-10-23 |
Family
ID=63844989
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810368415.2A Pending CN108689716A (en) | 2018-04-23 | 2018-04-23 | The preparation method of high thermal-conductivity aluminum nitride ceramics structural member |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108689716A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761617A (en) * | 2019-02-22 | 2019-05-17 | 福建臻璟新材料科技有限公司 | F-Ca-Lu doped aluminum nitride complex phase ceramic green compact and its preparation process |
| CN110628223A (en) * | 2019-11-01 | 2019-12-31 | 银川艾森达新材料发展有限公司 | Heat-conducting filler |
| CN112811909A (en) * | 2021-01-06 | 2021-05-18 | 北京科技大学 | Method for preparing high-strength high-thermal-conductivity aluminum nitride through hot-pressing sintering |
| CN114655938A (en) * | 2022-05-23 | 2022-06-24 | 苏州锦艺新材料科技股份有限公司 | Preparation method of spherical aluminum nitride granulation powder and filler powder |
| CN116854481A (en) * | 2023-06-29 | 2023-10-10 | 北京科技大学 | Method for rapidly preparing high-heat-conductivity aluminum nitride ceramics with complex shape at low temperature |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1130607A (en) * | 1995-11-17 | 1996-09-11 | 清华大学 | Method for manufacturing high-heat conductivity aluminium nitride ceramics |
| CN1221711A (en) * | 1998-11-26 | 1999-07-07 | 河北工业大学 | Method of mfg. high thermal conductivity integrated circuit aluminum nitride ceramic substrate by curtain coating process |
| CN102030538A (en) * | 2009-09-30 | 2011-04-27 | 比亚迪股份有限公司 | Production method of aluminum nitride ceramic and aluminum nitride ceramic prepared by same |
| CN107188567A (en) * | 2017-06-12 | 2017-09-22 | 北京钢研新冶精特科技有限公司 | A kind of preparation method of high-heat conductivity aluminium nitride ceramics |
-
2018
- 2018-04-23 CN CN201810368415.2A patent/CN108689716A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1130607A (en) * | 1995-11-17 | 1996-09-11 | 清华大学 | Method for manufacturing high-heat conductivity aluminium nitride ceramics |
| CN1221711A (en) * | 1998-11-26 | 1999-07-07 | 河北工业大学 | Method of mfg. high thermal conductivity integrated circuit aluminum nitride ceramic substrate by curtain coating process |
| CN102030538A (en) * | 2009-09-30 | 2011-04-27 | 比亚迪股份有限公司 | Production method of aluminum nitride ceramic and aluminum nitride ceramic prepared by same |
| CN107188567A (en) * | 2017-06-12 | 2017-09-22 | 北京钢研新冶精特科技有限公司 | A kind of preparation method of high-heat conductivity aluminium nitride ceramics |
Non-Patent Citations (3)
| Title |
|---|
| 唐婕: "《环保陶瓷生产与应用》", 31 January 2018, 中国建材工业出版社 * |
| 李栋: "《建筑装饰装修施工技术》", 30 June 2013, 厦门大学出版社 * |
| 李红强: "《胶粘原理、技术及应用》", 31 January 2014, 华南理工大学出版社 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761617A (en) * | 2019-02-22 | 2019-05-17 | 福建臻璟新材料科技有限公司 | F-Ca-Lu doped aluminum nitride complex phase ceramic green compact and its preparation process |
| CN109761617B (en) * | 2019-02-22 | 2021-11-05 | 福建臻璟新材料科技有限公司 | F-Ca-Lu doped aluminum nitride complex phase ceramic green body and preparation process thereof |
| CN110628223A (en) * | 2019-11-01 | 2019-12-31 | 银川艾森达新材料发展有限公司 | Heat-conducting filler |
| CN112811909A (en) * | 2021-01-06 | 2021-05-18 | 北京科技大学 | Method for preparing high-strength high-thermal-conductivity aluminum nitride through hot-pressing sintering |
| CN114655938A (en) * | 2022-05-23 | 2022-06-24 | 苏州锦艺新材料科技股份有限公司 | Preparation method of spherical aluminum nitride granulation powder and filler powder |
| CN116854481A (en) * | 2023-06-29 | 2023-10-10 | 北京科技大学 | Method for rapidly preparing high-heat-conductivity aluminum nitride ceramics with complex shape at low temperature |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108689716A (en) | The preparation method of high thermal-conductivity aluminum nitride ceramics structural member | |
| CN106478105B (en) | A kind of method that multistep reaction sintering process prepares the thyrite of low residual silicon | |
| CN114149260B (en) | Low-thermal-conductivity high-entropy ceramic thermal barrier coating material | |
| Sun et al. | Fabrication of transparent Y2O3 ceramics via aqueous gelcasting | |
| CN107892576B (en) | Silicon carbide ceramic and preparation method thereof, and radiating fin and application thereof | |
| CN110655407A (en) | Preparation method of silicon carbide ceramic with controllable resistance | |
| JP2002201075A (en) | Silicon nitride ceramic substrate and silicon nitride ceramic circuit substrate using it and its manufacturing method | |
| CN109553419A (en) | A kind of air pressure solid-phase sintering boron carbide complex phase ceramic and preparation method thereof | |
| CN102070341A (en) | Preparation method for microwave solid-state synthesis of self-toughening silicon nitride ceramic | |
| WO2022156637A1 (en) | Method for preparing silicon nitride ceramic material | |
| CN106966700A (en) | A kind of short route preparation technology of tin indium oxide sintered body | |
| CN109627014A (en) | A kind of high-intensitive, high-termal conductivity Si3N4Ceramic material and preparation method thereof | |
| CN107200587B (en) | Preparation method of aluminum nitride matrix fluorescent ceramic and related fluorescent ceramic | |
| CN113354418B (en) | High-performance aluminum nitride ceramic substrate prepared by vacuum hot-pressing sintering method and preparation method | |
| CN112209722A (en) | Silicon nitride composite material, preparation method thereof and heating element | |
| CN116283251B (en) | Alumina ceramic and preparation method and application thereof | |
| CN104230344A (en) | Low-temperature sintering preparation method of AlN ceramic added with multi-element sintering aid | |
| CN107200589B (en) | Preparation method of aluminum nitride matrix fluorescent ceramic and related fluorescent ceramic | |
| CN110759733B (en) | Y0.5Dy0.5Ta0.5Nb0.5O4Tantalum ceramic material and preparation method thereof | |
| CN105622102B (en) | Class boron carbide phase silicon carbide or class boron carbide phase silicon carbide boron carbide diphase ceramic material and preparation method thereof | |
| CN113735569B (en) | Preparation method of magnesium oxide and boron nitride composite microspheres | |
| CN109761618A (en) | A kind of high-densit boron carbide enhancing Aluminum nitride composite ceramic preparation method | |
| CN103539457A (en) | Preparation method of AlN ceramic base plate for microelectronic packaging | |
| CN113213936A (en) | Preparation method of ceramic powder doped modified self-sintered graphite composite material | |
| WO2017157157A1 (en) | Method for preparing fluorescent ceramic provided with aluminum nitride substrate, and related fluorescent ceramic |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181023 |
|
| RJ01 | Rejection of invention patent application after publication |