CN108706980A - Aluminium nitride ceramics and preparation method thereof, electrostatic chuck and application - Google Patents
Aluminium nitride ceramics and preparation method thereof, electrostatic chuck and application Download PDFInfo
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- CN108706980A CN108706980A CN201810681428.5A CN201810681428A CN108706980A CN 108706980 A CN108706980 A CN 108706980A CN 201810681428 A CN201810681428 A CN 201810681428A CN 108706980 A CN108706980 A CN 108706980A
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- 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
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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Abstract
The present invention relates to a kind of aluminium nitride ceramics and preparation method thereof, electrostatic chuck and applications.A kind of preparation method of aluminium nitride ceramics, includes the following steps：Raw material is mixed to get mixture, wherein, raw material includes aluminum nitride powder and sintering aid, according to mass percentage meter, the median that aluminum nitride powder includes 70%~80% is 0.5 micron~2 microns of the first aluminum nitride particle and 20%~30% median is 6 microns~8 microns the second aluminum nitride particle；Mixture is molded, green body is obtained；Green body is sintered in a reducing atmosphere, obtains aluminium nitride ceramics.The aluminium nitride ceramics that the above method is prepared has preferable thermal conductivity.
Description
Technical field
The present invention relates to ceramic material fields, more particularly to a kind of aluminium nitride ceramics and preparation method thereof, electrostatic chuck
And application.
Background technology
In traditional semiconductor wafer and liquid crystal display manufacturing process, vacuum cup or mechanical chuck are generally used
Carry out fixed wafer.Due to using in mechanical chuck fixed wafer process, often due to the effects that pressure, friction, collision
Wafer damage can be caused, or even easily leads to corrosion under that there is also effective working (finishing) areas is small, conductivity of heat is poor and plasma bombardment
The defects of grain deposition.And vacuum cup is there are heat-transfer capability is poor, and the defects of cannot work under vacuum conditions, thus greatly
Ground limits it and uses field.And novel electrostatic chuck ceramics can be using electrostatic attraction come fixed wafer, preferable dielectric
The desorption response of preferable adsorption capacity and treated object may be implemented in constant, volume resistivity, resistance to pressure etc..
AlN is because with high heat conductance, low-k, low-dielectric loss, having with Si the linear expansion coefficient to match, exhausted
Edge, mechanical performance etc., and as the first choice of electrostatic chuck material of new generation.However, there is lead for current aluminium nitride ceramics
The relatively low problem of heating rate, and affect its development.
Invention content
Based on this, it is necessary to provide a kind of preparation method of the preferable aluminium nitride ceramics of thermal conductivity.
In addition, also providing a kind of aluminium nitride ceramics, electrostatic chuck and application.
A kind of preparation method of aluminium nitride ceramics, includes the following steps：
Raw material is mixed to get mixture, wherein the raw material includes aluminum nitride powder and sintering aid, is contained according to quality percentage
Gauge, the aluminum nitride powder include 70%~80% median be 0.5 micron~2 microns the first aluminum nitride particle and
The second aluminum nitride particle that 20%~30% median is 6 microns~8 microns；
The mixture is molded, green body is obtained；And
The green body is sintered in a reducing atmosphere, obtains aluminium nitride ceramics.
The reducing atmosphere is mixed to form by reducibility gas and protective gas in one of the embodiments, described to go back
The mass ratio of originality gas and the protective gas is 10~30:70~90.
The reducibility gas is selected from least one of carbon monoxide and hydrogen in one of the embodiments,.
The sintering aid is selected from lithia, sodium oxide molybdena, magnesia, niobium pentaoxide and oxygen in one of the embodiments,
Change at least one of calcium；And/or the mass ratio of the sintering aid and the aluminum nitride powder is 1:100~6:100.
Described the step of raw material is mixed to get mixture, includes in one of the embodiments,：By the sintering aid and
The aluminum nitride powder is mixed by dry ball milling, then through drying, is crossed 300 mesh and sieved~400 mesh sieve, obtain the mixture.
The method that the green body is sintered in a reducing atmosphere is microwave sintering in one of the embodiments,；And/
Or, the sintering temperature that the green body is sintered in a reducing atmosphere is 1600 DEG C~1800 DEG C.
First aluminum nitride particle and second aluminum nitride particle are spherical shape in one of the embodiments,.
A kind of aluminium nitride ceramics is prepared by the preparation method of any of the above-described kind of aluminium nitride ceramics.
A kind of electrostatic chuck is obtained by above-mentioned aluminium nitride ceramics working process.
Application of the above-mentioned electrostatic chuck in the working process of wafer.
The preparation method of above-mentioned aluminium nitride ceramics is 0.5 micron~2 by using including 70%~80% median
The nitrogen for the second aluminum nitride particle that first aluminum nitride particle of micron and 20%~30% median are 6 microns~8 microns
Change aluminium powder is raw material, to be fabricated to green body by the aluminum nitride particle mixed-forming of different-grain diameter, so that the particle packing of green body
It is more close, to improve the consistency of aluminium nitride ceramics；Meanwhile addition sintering aid can promote the sintering of aluminum nitride powder, to carry
The densification of high aluminium nitride ceramics improves the thermal conductivity of aluminium nitride ceramics；And by the way that green body to be sintered in a reducing atmosphere, so that
Reduction reaction can occur in a reducing atmosphere for the impurity oxygen in aln surface and lattice, and reach removal aln surface and
The purpose of oxygen in aluminium nitride lattice improves aluminium nitride perfection of lattice in sintering process, reduces the formation in aluminium vacancy, to
Improve the thermal conductivity of aluminium nitride ceramics.
Description of the drawings
Fig. 1 is the flow chart of the preparation method of the aluminium nitride ceramics of an embodiment.
Specific implementation mode
To facilitate the understanding of the present invention, below with reference to relevant drawings to invention is more fully described.In attached drawing
Give the preferred embodiment of the present invention.But the present invention can realize in many different forms, however it is not limited to herein
Described embodiment.Keep the understanding to the disclosure more saturating on the contrary, purpose of providing these embodiments is
It is thorough comprehensive.
Unless otherwise defined, all of technologies and scientific terms used here by the article and belong to the technical field of the present invention
The normally understood meaning of technical staff is identical.Used term is intended merely to description tool in the description of the invention herein
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term " and or " used herein includes one or more phases
Any and all combinations of the Listed Items of pass.
As shown in Figure 1, the preparation method of the aluminium nitride ceramics of an embodiment, includes the following steps：
Step S110：Raw material is mixed to get mixture.
Wherein, raw material includes aluminium nitride (AlN) powder and sintering aid, and according to mass percentage meter, aluminum nitride powder includes
70%~80% median is 0.5 micron~2 microns of the first aluminum nitride particle and 20%~30% median is 6
Micron~8 microns of the second aluminum nitride particle.
Further, the first aluminum nitride particle and the second aluminum nitride particle are spherical shape.Spherical aluminum nitride particle has
Preferable mobility can obtain more uniform mixture during mixing, and spherical aluminum nitride particle is conducive to
The densification of aluminium nitride reduces the defect of aluminium nitride, further increases intensity, the thermal conductivity of aluminium nitride ceramics, and makes entire nitrogen
Changing aluminium ceramics has more uniform thermal conductivity and intensity.
Sintering aid is that can generate the inorganic matter of liquid phase with oxidation reactive aluminum in sintering process.Further, sintering aid
Selected from least one of lithia, sodium oxide molybdena, magnesia, niobium pentaoxide and calcium oxide.These sintering aids can be with nitridation
Oxidation reactive aluminum in aluminium generates aluminate, forms liquid-phase sintering at a lower temperature, can not only reduce the burning of aluminium nitride
Junction temperature, and the aluminate generated volatilizees at 1350 DEG C or so, moreover it is possible to the lattice defect of aluminium nitride is reduced, aluminium nitride pottery is improved
The thermal conductivity of porcelain.Further, sintering aid is lithia, and lithia has better wetability to aluminium oxide, can be more preferable
Ground and the oxidation reactive aluminum in aluminium nitride, can more reduce the lattice defect of aluminium oxide.
The mass ratio of sintering aid and aluminum nitride powder is 1 in one of the embodiments,:100~6:100.The proportioning helps
The sintering of aluminium nitride can not only be promoted by burning agent, reduce sintering temperature, but also can make aluminium nitride ceramics while have higher
Consistency, preferable thermal conductivity and mechanical strength.
Raw material is made of aluminium nitride (AlN) powder and sintering aid in one of the embodiments, and aluminium nitride is by 70%~80%
Median be 0.5 micron~2 microns of the first aluminum nitride particle and 20%~30% median is 6 microns~8 micro-
The second aluminum nitride particle composition of rice, sintering aid is lithia, and the mass ratio of sintering aid and aluminum nitride powder is 1:100~6:
100.The raw material of the formula can make silicon nitride ceramics have more excellent heat conductivility, higher consistency, higher strong
Degree, lower dielectric constant and lower electrical loss.
The step of raw material is mixed to get mixture in one of the embodiments, include：By sintering aid and aluminum nitride powder
It is mixed by dry ball milling, then through drying, crosses 300 mesh and sieve~400 mesh sieve, obtain mixture.
The mixed drying steps of dry ball milling are in one of the embodiments,：Dry 12 is small at 40 DEG C~70 DEG C
When~24 hours, to remove water in mixture, because in dry ball milling, mixture has the possibility for absorbing the water in air
Property.
The time of dry ball milling mixing is 48 hours~96 hours in one of the embodiments,.
Further, further include by sintering aid before the step of sintering aid and aluminum nitride powder being mixed by dry ball milling
The step of 12 hours~24 hours dry at 40 DEG C~70 DEG C with aluminum nitride powder.By the way that powder is dried before and after ball milling,
To remove the water in powder, powder water suction and sodium oxide molybdena, potassium oxide vigorous reaction are prevented, the performance of aluminium nitride is influenced.
It should be noted that the step of raw material is mixed to get mixture is not limited to the side of above-mentioned dry ball milling mixing
Formula, can also by the way of wet ball grinding, at this point it is possible to using anhydrous organic matter as solvent, such as absolute ethyl alcohol or
Water, if water as solvent, and when having used a kind of in lithia and sodium oxide molybdena as sintering aid, need first by lithia and/
Or sodium oxide molybdena first incorporates in water, becomes sodium hydroxide, lithium hydroxide, because this process is highly exothermic, reaction is violent, adds
Into powder, the ball milling together with other sintering aids is sintered lithium hydroxide at high temperature, sodium hydroxide becomes lithia again, oxidation
Sodium, to continue to play the role of sintering aid.And dry ball milling mixing can prevent lithia, sodium oxide molybdena and solvent reaction and introduce
Other impurity.
Step S120：Mixture is molded, green body is obtained.
Specifically, it is dry-pressing or cold isostatic compaction by the molding method of mixture.
Step S130：Green body is sintered in a reducing atmosphere, obtains aluminium nitride ceramics.
By the way that green body to be sintered in a reducing atmosphere, so that the impurity oxygen energy in the oxygen of aln surface and aluminium nitride lattice
It is enough that reduction reaction occurs in a reducing atmosphere, and achieve the purpose that remove oxygen in aln surface and aluminium nitride lattice, improve nitrogen
Change aluminium perfection of lattice in sintering process, the formation in aluminium vacancy is reduced, to improve the thermal conductivity of aluminium nitride ceramics.
Reducing atmosphere is mixed to form by reducibility gas and protective gas in one of the embodiments, and reproducibility gas
The mass ratio of body and protective gas is 10~30:70~90, which can not only reach removal aln surface and nitrogen
Change the purpose of oxygen in aluminium lattice, and can also ensure that the safety of reaction process.It should be noted that other be embodiment
In, reducing atmosphere can also be made of reducibility gas.
Reducibility gas is selected from least one of carbon monoxide and hydrogen in one of the embodiments,.Further,
Reducibility gas is carbon monoxide, and carbon monoxide has better affinity to the impurity oxygen in aln surface and lattice, more
The oxygen content in aluminium nitride is advantageously reduced, can better ensure that aluminium nitride perfection of lattice.Protective gas be nitrogen or
Argon gas.
The method that green body is sintered in a reducing atmosphere in one of the embodiments, is microwave sintering, by restoring
Microwave sintering is carried out in atmosphere can improve the thermal conductivity of entire aluminium nitride ceramics and the homogeneity of intensity, in general electrostatic chuck
Face is coated with one layer of circuit, this layer of circuit can determine whether certain places heat according to the temperature difference on surface, and thermal conductivity is uneven
One or thermal conductivity it is low, it will influence the homogeneity of the surface temperature of electrostatic chuck, and then influence the use quality of electrostatic chuck.
Specifically, sintering temperature is 1600 DEG C~1800 DEG C.Sintering time is 1 hour~4 hours.
The preparation method of above-mentioned aluminium nitride ceramics at least has the advantage that：
For aluminium nitride as a kind of covalent compound, fusing point is high, self-diffusion coefficient is small, is caused therefore, it is necessary to complete at high temperature
Densification is sintered, and since aluminium nitride has stronger affinity to oxygen, part oxygen can be dissolved into the lattice of aluminium nitride at high temperature,
To form aluminium vacancy, generates aluminium vacancy and scatter phonon, reduce the mean free path of phonon, decline so as to cause thermal conductivity, and
The preparation method of above-mentioned aluminium nitride ceramics is by using including 70%~80% median is 0.5 micron~2 microns the
One aluminum nitride particle and 20%~30% median be 6 microns~8 microns the aluminum nitride powder of the second aluminum nitride particle be
Raw material, to be fabricated to green body by the aluminum nitride particle mixed-forming of different-grain diameter, so that the particle packing of green body is more close,
To improve the consistency of aluminium nitride ceramics；Meanwhile addition sintering aid can promote the sintering of aluminum nitride powder, to improve aluminium nitride pottery
The densification of porcelain improves the thermal conductivity of aluminium nitride ceramics；And by the way that green body to be sintered in a reducing atmosphere, so that aln surface
Reduction reaction can occur in a reducing atmosphere with the impurity oxygen in lattice, and reach removal aln surface and aluminium nitride lattice
The purpose of middle oxygen improves aluminium nitride perfection of lattice in sintering process, the formation in aluminium vacancy is reduced, to improve aluminium nitride
The thermal conductivity of ceramics.Meanwhile the high densification degree of aluminium nitride ceramics and less aluminium vacancy so that aluminium nitride ceramics also has
Higher intensity.
Since electrostatic chuck is used in the environment of plasma, in the environment of high energy plasma bombardment, this two
Performance be weigh whether resistant to plasma bombardment performance indicator, if this two performances are not up to standard, service life can be very low, and
The experiment proved that the aluminium nitride ceramics that the preparation method of above-mentioned aluminium nitride ceramics is prepared also have both lower dielectric constant and
Lower electrical loss has preferable insulation performance.
The aluminium nitride ceramics of one embodiment is prepared by the preparation method of above-mentioned aluminium nitride ceramics so that the nitridation
Aluminium ceramics not only have higher thermal conductivity and higher consistency, meanwhile, also there is higher intensity, lower dielectric constant
With lower electrical loss.
The electrostatic chuck of one embodiment is obtained by above-mentioned aluminium nitride ceramics working process.Due to above-mentioned aluminium nitride ceramics
Not only there is higher thermal conductivity and higher consistency, meanwhile, also there is higher intensity, higher homogeneity, lower
Dielectric constant and lower electrical loss, therefore, the electrostatic chuck also not only have higher thermal conductivity and higher consistency, together
When, also there is higher intensity, lower dielectric constant and lower electrical loss.
Include in one of the embodiments, following step by the method that aluminium nitride ceramics working process obtains electrostatic chuck
Suddenly：Slot electrode is formed on aluminium nitride ceramics, is then formed electrode green body layer in slot electrode, will be formed with electrode green body layer
Aluminium nitride ceramics cofiring at 1000 DEG C~1400 DEG C, obtains electrostatic chuck.
The method for forming electrode layer in slot electrode in one of the embodiments, is silk-screen printing；The material of electrode layer
For the electrocondution slurry containing molybdenum and manganese.Specifically, further include to nitridation before the step of forming slot electrode on aluminium nitride ceramics
The step of aluminium ceramics are polished.
The method for forming slot electrode on aluminium nitride ceramics in one of the embodiments, is plasma etching.
Above-mentioned electrostatic chuck can be in the application in the working process of wafer, for fixing wafer, due to above-mentioned electrostatic card
Disk has preferable thermal conductivity so that wafer can more uniformly be heated in process, be conducive to improve adding for wafer
Work yield and quality.
It is that (following embodiment unless otherwise specified, does not then contain and remove inevitable impurity specific embodiment part below
Other components not yet explicitly pointed out in addition.)：
Embodiment 1
The preparation process of the aluminium nitride ceramics of the present embodiment is as follows：
(1) raw material is weighed, raw material is made of spherical aluminum nitride powder and sintering aid, according to mass percentage meter, nitridation
Aluminium powder is by the second nitridation that the median of the first aluminum nitride particle that 75% median is 1 micron and 25% is 7 microns
Alumina particles form, and sintering aid is lithia, and the mass ratio of sintering aid and aluminum nitride powder is 4:100.
(2) sintering aid and aluminum nitride powder is 18 hours dry at 55 DEG C, then dry ball milling mixes 72 hours, then 55
It is 18 hours dry at DEG C, 350 mesh sieve is then crossed, mixture is obtained.
(3) mixture is dry-pressing formed, obtain green body.
(4) in the atmosphere of the mixed gas of carbon monoxide and nitrogen, by green body at 1700 DEG C microwave sintering 2 hours,
Obtain aluminium nitride ceramics, wherein the mass ratio of carbon monoxide and nitrogen is 20:80.
Embodiment 2
The preparation process of the aluminium nitride ceramics of the present embodiment is as follows：
(1) raw material is weighed, raw material is made of spherical aluminum nitride powder and sintering aid, according to mass percentage meter, nitridation
Aluminium powder is by the second nitridation that the median of the first aluminum nitride particle that 70% median is 2 microns and 30% is 6 microns
Alumina particles form, and sintering aid is lithia, and the mass ratio of sintering aid and aluminum nitride powder is 1:100.
(2) sintering aid and aluminum nitride powder is 24 hours dry at 40 DEG C, then dry ball milling mixes 96 hours, then 40
It is 24 hours dry at DEG C, 300 mesh sieve is then crossed, mixture is obtained.
(3) mixture is dry-pressing formed, obtain green body.
(4) in the atmosphere of the mixed gas of carbon monoxide and nitrogen, by green body at 1600 DEG C microwave sintering 4 hours,
Obtain aluminium nitride ceramics, wherein the mass ratio of carbon monoxide and nitrogen is 10:90.
Embodiment 3
The preparation process of the aluminium nitride ceramics of the present embodiment is as follows：
(1) raw material is weighed, raw material is made of spherical aluminum nitride powder and sintering aid, according to mass percentage meter, nitridation
The second nitrogen that aluminium powder is 8 microns by the median of the first aluminum nitride particle that 80% median is 0.5 micron and 20%
Change alumina particles composition, sintering aid is lithia, and the mass ratio of sintering aid and aluminum nitride powder is 6:100.
(2) sintering aid and aluminum nitride powder is 12 hours dry at 70 DEG C, then dry ball milling mixes 48 hours, then 70
It is 12 hours dry at DEG C, 400 mesh sieve is then crossed, mixture is obtained.
(3) mixture is dry-pressing formed, obtain green body.
(4) in the atmosphere of the mixed gas of carbon monoxide and argon gas, by green body at 1800 DEG C microwave sintering 1 hour,
Obtain aluminium nitride ceramics, wherein the mass ratio of carbon monoxide and argon gas is 30:70.
Embodiment 4
The preparation process of the aluminium nitride ceramics of the present embodiment is as follows：
(1) raw material is weighed, raw material is made of spherical aluminum nitride powder and sintering aid, according to mass percentage meter, nitridation
Aluminium powder is by second that the median of the first aluminum nitride particle that 75% median is 1.5 microns and 30% is 6.5 microns
Aluminum nitride particle forms, and sintering aid is lithia, and the mass ratio of sintering aid and aluminum nitride powder is 2:100.
(2) sintering aid and aluminum nitride powder is 20 hours dry at 50 DEG C, then dry ball milling mixes 80 hours, then 50
It is 20 hours dry at DEG C, 300 mesh sieve is then crossed, mixture is obtained.
(3) by mixture cold isostatic pressing, green body is obtained.
(4) in the atmosphere of the mixed gas of carbon monoxide and nitrogen, by green body at 1700 DEG C microwave sintering 3 hours,
Obtain aluminium nitride ceramics, wherein the mass ratio of carbon monoxide and nitrogen is 15:85.
Embodiment 5
The preparation process of the aluminium nitride ceramics of the present embodiment is as follows：
(1) raw material is weighed, raw material is made of spherical aluminum nitride powder and sintering aid, according to mass percentage meter, nitridation
Aluminium powder is by the second nitridation that the median of the first aluminum nitride particle that 78% median is 1 micron and 22% is 8 microns
Alumina particles form, and sintering aid is lithia, and the mass ratio of sintering aid and aluminum nitride powder is 5:100.
(2) sintering aid and aluminum nitride powder is 18 hours dry at 60 DEG C, then dry ball milling mixes 90 hours, then 65
It is 15 hours dry at DEG C, 400 mesh sieve is then crossed, mixture is obtained.
(3) by mixture cold isostatic pressing, green body is obtained.
(4) in the atmosphere of the mixed gas of carbon monoxide and nitrogen, by green body, microwave sintering 3.5 is small at 1650 DEG C
When, obtain aluminium nitride ceramics, wherein the mass ratio of carbon monoxide and nitrogen is 25:75.
Embodiment 6
The preparation process of the aluminium nitride ceramics of the present embodiment is as follows：
(1) raw material is weighed, raw material is made of spherical aluminum nitride powder and sintering aid, according to mass percentage meter, nitridation
Aluminium powder is by the second nitridation that the median of the first aluminum nitride particle that 75% median is 2 microns and 25% is 7 microns
Alumina particles form, and sintering aid is lithia, and the mass ratio of sintering aid and aluminum nitride powder is 3:100.
(2) sintering aid and aluminum nitride powder is 22 hours dry at 45 DEG C, then dry ball milling mixes 65 hours, then 50
It is 20 hours dry at DEG C, 350 mesh sieve is then crossed, mixture is obtained.
(3) by mixture cold isostatic pressing, green body is obtained.
(4) in the atmosphere of the mixed gas of carbon monoxide and argon gas, by green body, microwave sintering 1.5 is small at 1750 DEG C
When, obtain aluminium nitride ceramics, wherein the mass ratio of carbon monoxide and argon gas is 22:78.
Embodiment 7
The preparation process substantially phase of the preparation process of the aluminium nitride ceramics of the present embodiment and the aluminium nitride ceramics of embodiment 1
Together, difference lies in the sintering aid of the present embodiment is different from embodiment 1, and the sintering aid of the present embodiment is sodium oxide molybdena.
Embodiment 8
The preparation process substantially phase of the preparation process of the aluminium nitride ceramics of the present embodiment and the aluminium nitride ceramics of embodiment 1
Together, difference lies in the sintering aid of the present embodiment is different from embodiment 1, and the sintering aid of the present embodiment is 1 by mass ratio:1 oxidation
Lithium and magnesia composition.
Embodiment 9
The preparation process substantially phase of the preparation process of the aluminium nitride ceramics of the present embodiment and the aluminium nitride ceramics of embodiment 1
Together, difference lies in the sintering aid of the present embodiment is different from embodiment 1, and the sintering aid of the present embodiment is 1 by mass ratio:1:1 oxygen
Change lithium, sodium oxide molybdena and calcium oxide composition.
Embodiment 10
The preparation process substantially phase of the preparation process of the aluminium nitride ceramics of the present embodiment and the aluminium nitride ceramics of embodiment 1
Together, difference lies in the sintering aid of the present embodiment is different from embodiment 1, and the sintering aid of the present embodiment is 1 by mass ratio:1:1 oxygen
Change lithium, sodium oxide molybdena, niobium pentaoxide and calcium oxide composition.
Embodiment 11
The preparation process substantially phase of the preparation process of the aluminium nitride ceramics of the present embodiment and the aluminium nitride ceramics of embodiment 1
Together, difference lies in the sintering aid of the present embodiment is different from embodiment 1, and the sintering aid of the present embodiment is 1 by mass ratio:1:1:1:1
Lithia, sodium oxide molybdena, magnesia, niobium pentaoxide and calcium oxide composition.
Embodiment 12
The preparation process substantially phase of the preparation process of the aluminium nitride ceramics of the present embodiment and the aluminium nitride ceramics of embodiment 1
Together, difference lies in the sintering aid of the present embodiment is different from embodiment 1, and the sintering aid of the present embodiment is 1 by mass ratio:1:1:1
Sodium oxide molybdena, magnesia, niobium pentaoxide and calcium oxide composition.
Embodiment 13
The preparation process substantially phase of the preparation process of the aluminium nitride ceramics of the present embodiment and the aluminium nitride ceramics of embodiment 1
Together, difference lies in the sintering aid of the present embodiment is different from embodiment 1, and the sintering aid of the present embodiment is 1 by mass ratio:1:1 oxygen
Change magnesium, niobium pentaoxide and calcium oxide composition.
Embodiment 14
The preparation process substantially phase of the preparation process of the aluminium nitride ceramics of the present embodiment and the aluminium nitride ceramics of embodiment 1
Together, the step of sintering processing of the step of difference lies in, the present embodiment (4) is different, the present embodiment (4) are：By green body full of
It is sintered 2 hours at 1700 DEG C in the furnace body of the mixed gas of carbon monoxide and nitrogen.
Embodiment 15
The preparation process substantially phase of the preparation process of the aluminium nitride ceramics of the present embodiment and the aluminium nitride ceramics of embodiment 1
Together, difference lies in the sintering aid of the present embodiment and the mass ratio of aluminum nitride powder are 0.5:100.
Embodiment 16
The preparation process substantially phase of the preparation process of the aluminium nitride ceramics of the present embodiment and the aluminium nitride ceramics of embodiment 1
Together, difference lies in the sintering aid of the present embodiment and the mass ratio of aluminum nitride powder are 7:100.
Embodiment 17
The preparation process substantially phase of the preparation process of the aluminium nitride ceramics of the present embodiment and the aluminium nitride ceramics of embodiment 1
Together, the step of difference lies in, the present embodiment (4) is the progress microwave sintering in the atmosphere of the mixed gas of hydrogen and nitrogen,
Wherein, the mass ratio of hydrogen and nitrogen is 20:80.
Embodiment 18
The preparation process substantially phase of the preparation process of the aluminium nitride ceramics of the present embodiment and the aluminium nitride ceramics of embodiment 1
Together, difference lies in the sintering aid of the present embodiment is sodium oxide molybdena, and step (4) is the atmosphere in the mixed gas of hydrogen and nitrogen
Middle progress microwave sintering, wherein the mass ratio of hydrogen and nitrogen is 20:80.
Embodiment 19
The preparation process substantially phase of the preparation process of the aluminium nitride ceramics of the present embodiment and the aluminium nitride ceramics of embodiment 1
Together, the step of difference lies in, the present embodiment (4) be carried out in the atmosphere of the mixed gas of hydrogen, carbon monoxide and nitrogen it is micro-
Wave sintering, wherein the mass ratio of hydrogen and carbon monoxide is 1:1, the matter of the quality sum and nitrogen of hydrogen and carbon monoxide
Amount is than being 20:80.
Embodiment 20
The preparation process substantially phase of the preparation process of the aluminium nitride ceramics of the present embodiment and the aluminium nitride ceramics of embodiment 1
Together, it is 1 that difference lies in the sintering aids of, the present embodiment by mass ratio:1:1:1:1 lithia, sodium oxide molybdena, magnesia, five oxidations
Two niobiums and calcium oxide composition, and step (4) is the progress microwave burning in the atmosphere of the mixed gas of hydrogen, carbon monoxide and nitrogen
Knot, wherein the mass ratio of hydrogen and carbon monoxide is 1:1, the mass ratio of the quality sum and nitrogen of hydrogen and carbon monoxide
It is 20:80.
Comparative example 1
The preparation process of the aluminium nitride ceramics of comparative example 1 is roughly the same with the preparation process of the aluminium nitride ceramics of embodiment 1,
The aluminum nitride particle composition that the median that aluminum nitride powder difference lies in, comparative example 1 is 100% is 1 micron.
Comparative example 2
The preparation process of the aluminium nitride ceramics of comparative example 2 is roughly the same with the preparation process of the aluminium nitride ceramics of embodiment 1,
The second aluminum nitride particle composition that the median that aluminum nitride powder difference lies in, comparative example 2 is 100% is 7 microns.
Comparative example 3
The preparation process of the aluminium nitride ceramics of comparative example 3 is roughly the same with the preparation process of the aluminium nitride ceramics of embodiment 1,
It is 1 micron of the first aluminum nitride particle and 15% middle position that difference lies in the aluminum nitride powders of, comparative example 3 by 85% median
The second aluminum nitride particle that grain size is 7 microns forms.
Comparative example 4
The preparation process of the aluminium nitride ceramics of comparative example 4 is roughly the same with the preparation process of the aluminium nitride ceramics of embodiment 1,
It is 1 micron of the first aluminum nitride particle and 40% middle position that difference lies in the aluminum nitride powders of, comparative example 4 by 60% median
The second aluminum nitride particle that grain size is 7 microns forms.
Comparative example 5
The preparation process of the aluminium nitride ceramics of comparative example 5 is roughly the same with the preparation process of the aluminium nitride ceramics of embodiment 1,
The step of difference lies in, comparative example 5 (4) be nitrogen atmosphere in carry out microwave sintering.
Test：
The densification of the aluminium nitride ceramics of testing example 1~20 and comparative example 1~5 is distinguished according to Archimedes's drainage
Degree；The intensity of the aluminium nitride ceramics of testing example 1~20 and comparative example 1~5 is distinguished according to three-point bending test；Using laser
Flicker method distinguishes the thermal conductivity of the aluminium nitride ceramics of testing example 1~20 and comparative example 1~5；According to concentration circuit method method
The dielectric constant and dielectric loss of the aluminium nitride ceramics of testing example 1~20 and comparative example 1~5 respectively.
The aluminium nitride ceramics of Examples 1 to 20 and comparative example 1~5 is polished, then lost in aluminium nitride ceramics upper plasma
Form slot electrode quarter, then screen printing scopiform will be formed with electrode green body layer at molybdenum manganese alloy electrode green body layer in slot electrode
Aluminium nitride ceramics at 1200 DEG C cofiring, obtain electrostatic chuck.Using laser flash method testing example 1~20 and comparative example
Thermal conductivity value of the electrostatic chuck that 1~5 aluminium nitride ceramics is prepared on different location, to weigh the uniform of electrostatic chuck
Property, value is bigger, and homogeneity is poorer, it is better to be worth smaller homogeneity, wherein homogeneity=(maximum thermal conductivity value-minimum thermal conductivity value)
× 100%/maximum thermal conductivity value.
Wherein, consistency, intensity, thermal conductivity, the dielectric of the aluminium nitride ceramics of Examples 1 to 20 and comparative example 1~5 are normal
Number, dielectric loss and homogeneity are shown in Table 1 respectively.
Table 1
From table 1 it follows that the thermal conductivity of the aluminium nitride ceramics of Examples 1 to 20 is at least 150w/mK, it is clear that
The significantly larger than thermal conductivity of the aluminium nitride ceramics of 1~comparative example of comparative example 5, and the densification of the aluminium nitride ceramics of Examples 1 to 20
Degree is at least 98.05%, and intensity is at least 370MPa, and dielectric constant is at most only 7.67C2/(N*M2), dielectric loss is up to
2.24×10-4KV/mm, also far superior to 1~comparative example of comparative example 5, meanwhile, the aluminium nitride ceramics of Examples 1 to 20 also has
More excellent homogeneity.
Each technical characteristic of embodiment described above can be combined arbitrarily, to keep description succinct, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, it is all considered to be the range of this specification record.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of preparation method of aluminium nitride ceramics, which is characterized in that include the following steps：
Raw material is mixed to get mixture, wherein the raw material includes aluminum nitride powder and sintering aid, according to mass percentage
Meter, the first aluminum nitride particle and 20% that the median that the aluminum nitride powder includes 70%~80% is 0.5 micron~2 microns
The second aluminum nitride particle that~30% median is 6 microns~8 microns；
The mixture is molded, green body is obtained；And
The green body is sintered in a reducing atmosphere, obtains aluminium nitride ceramics.
2. the preparation method of aluminium nitride ceramics according to claim 1, which is characterized in that the reducing atmosphere is by reproducibility
Gas and protective gas are mixed to form, and the mass ratio of the reducibility gas and the protective gas is 10~30:70~90.
3. the preparation method of aluminium nitride ceramics according to claim 2, which is characterized in that the reducibility gas is selected from one
At least one of carbonoxide and hydrogen.
4. the preparation method of aluminium nitride ceramics according to claim 1, which is characterized in that the sintering aid is selected from oxidation
At least one of lithium, sodium oxide molybdena, magnesia, niobium pentaoxide and calcium oxide；And/or the sintering aid and the aluminium nitride
The mass ratio of powder is 1:100~6:100.
5. the preparation method of aluminium nitride ceramics according to claim 1, which is characterized in that it is described raw material is mixed to get it is mixed
Closing the step of expecting includes：The sintering aid and the aluminum nitride powder are mixed by dry ball milling, then through drying, cross 300 mesh sieve
~400 mesh sieve, and obtain the mixture.
6. the preparation method of aluminium nitride ceramics according to claim 1, which is characterized in that described to restore the green body
The method being sintered in atmosphere is microwave sintering；And/or the sintering temperature for being sintered the green body in a reducing atmosphere is
1600 DEG C~1800 DEG C.
7. the preparation method of aluminium nitride ceramics according to claim 1, which is characterized in that first aluminum nitride particle and
Second aluminum nitride particle is spherical shape.
8. a kind of aluminium nitride ceramics, which is characterized in that by the preparation side of claim 1~7 any one of them aluminium nitride ceramics
Method is prepared.
9. a kind of electrostatic chuck, which is characterized in that obtained by aluminium nitride ceramics working process according to any one of claims 8.
10. application of the electrostatic chuck in the working process of wafer described in claim 9.
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| CN113773091A (en) * | 2021-08-11 | 2021-12-10 | 臻金新材(深圳)有限公司 | Aluminum nitride ceramic tape-casting slurry, aluminum nitride ceramic substrate and preparation method |
| CN113773091B (en) * | 2021-08-11 | 2023-10-24 | 臻金新材(深圳)有限公司 | Aluminum nitride ceramic casting slurry, aluminum nitride ceramic substrate and preparation method |
| CN116813352A (en) * | 2023-06-29 | 2023-09-29 | 中国电子科技集团公司第四十八研究所 | Aluminum nitride ceramic material and preparation method and application thereof |
| CN116813352B (en) * | 2023-06-29 | 2024-10-01 | 中国电子科技集团公司第四十八研究所 | Aluminum nitride ceramic material and preparation method and application thereof |
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