CN106187123A - Aluminium oxide ceramics and preparation method thereof and plasma etch apparatus - Google Patents
Aluminium oxide ceramics and preparation method thereof and plasma etch apparatus Download PDFInfo
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Abstract
The present invention relates to a kind of aluminium oxide ceramics and preparation method thereof.The preparation method of this aluminium oxide ceramics comprises the steps: to add water organic monomer, cross-linking agent and dispersant mixing, and regulates pH value to 9～10, obtains pre-mixing liquor；Nano alumina powder and inhibiting grain growth agent powder are joined in described pre-mixing liquor, blended, obtain the volumn concentration of solid phase be 35～45%, the viscosity ceramic size less than 1Pa s, wherein, the particle diameter of nano alumina powder is 5～40 nanometers, and the particle diameter of inhibiting grain growth agent powder is 5～50 nanometers；In ceramic size, add catalyst and initiator, through gelation, obtain wet base；Wet base is dried, more sintered, obtain aluminium oxide ceramics.The aluminium oxide ceramics that the preparation method of above-mentioned aluminium oxide ceramics prepares has preferable anti-plasma corrosive nature.
Description
Technical field
The present invention relates to ceramic material field, particularly relate to a kind of aluminium oxide ceramics and preparation method thereof and plasma
Etching apparatus.
Background technology
Plasma processing apparatus is widely used in semiconductor manufacturing, and it is mainly used in the techniques such as etching, surface clean.
Its operation principle is that the halide-containing gas ionizations such as CF4, C4F8 in reative cell are become plasma, and with in plasma
Free radical goes bombardment or sputters the surface molecular of the material that is etched, and forms volatile substances, thus realizes the purpose of etching.And it is anti-
The component in room is answered to expose in the plasma, by plasma etching in various degree, except reducing the use longevity of component
Ordering and increase the use cost of plasma processing apparatus, produced by plasma etching, metal/ceramic granule also can pollute
Reative cell and workpiece to be machined surface, affect the quality of workpiece to be machined.
In order to improve the anti-plasma corrosive nature of component, take kinds of processes measure, as sprayed at hardware
The inorganic matter coating such as yittrium oxide, aluminium oxide, but the coating of spraying is strong with the adhesion of hardware, and inorganic matter coating is with golden
The coefficient of expansion of metal elements does not mates, and in use there is the risk come off；As well as particles of inorganic material in coating
Being not reaching to sintering state, an interparticle cohesion is inadequate, easily comes off under plasma etching, it addition, the most useful sintering causes
Close ceramic material component, such as the ceramic material such as aluminium oxide, yittrium oxide, has certain in terms of anti-plasma corrosive nature
Promote, but some sintering aids added in the preparation process of the ceramic material such as aluminium oxide, yittrium oxide are easily rotten by plasma
Erosion, and ceramic material coarse grain of abnormal growth in sintering process both caused ceramic micro-structure bad be also easier to by
Plasma etching and come off, substantially reduce the service life of ceramic component, also can produce after being corroded of ceramic component meanwhile
The problem that raw ceramic particle pollutes processing workpiece.
Summary of the invention
Based on this, it is necessary to provide a kind of system that can prepare the preferable aluminium oxide ceramics of anti-plasma corrosive nature
Preparation Method.
Additionally, also provide for a kind of aluminium oxide ceramics and plasma etch apparatus.
The preparation method of a kind of aluminium oxide ceramics, comprises the steps:
Add water mixing by organic monomer, cross-linking agent and dispersant, and regulates pH value to 9～10, obtains pre-mixing liquor；
Nano alumina powder and inhibiting grain growth agent powder are joined in described pre-mixing liquor, blended, obtain solid phase
Volumn concentration be 35～45%, viscosity less than the ceramic size of 1Pa s, wherein, the particle diameter of described nano alumina powder is
5～40 nanometers, the particle diameter of described inhibiting grain growth agent powder is 5～50 nanometers；
In described ceramic size, add catalyst and initiator, through gelation, obtain wet base；
Described wet base is dried, more sintered, obtain aluminium oxide ceramics.
Wherein in an embodiment, described organic monomer is acrylamide, Methacrylamide or methylol acryloyl
Amine；Described cross-linking agent is N, N'-methylene-bisacrylamide；Described dispersant is selected from ammonium polyacrylate, ammonium citrate and poly-second
One in glycol.
Wherein in an embodiment, in described pre-mixing liquor, the weight/mass percentage composition of described organic monomer be 10～
20%, the weight/mass percentage composition of described dispersant is 2～5%, and described organic monomer is 10:1 with the mass ratio of described cross-linking agent
～40:1.
Wherein in an embodiment, described inhibiting grain growth agent powder with the mass ratio of described nano alumina powder is
0.5:100～1:100；At least one in magnesia powder and yttrium oxide powder of described inhibiting grain growth agent powder.
Wherein in an embodiment, described initiator is Ammonium persulfate., and described catalyst is N, N, N', N'-tetramethyl
Ethylenediamine.
Wherein in an embodiment, add in described ceramic size described catalyst and described initiator step it
Before, also include the step of described ceramic size evacuation de-bubble.
Wherein in an embodiment, by the step that described wet base is dried it is: described wet base is dried 1～5 at room temperature
My god, then it is incubated 10～20 hours in 90～100 DEG C.
Wherein in an embodiment, the step of described sintering is: the step of described sintering is: with 30～60 DEG C/h
Heating rate be warming up to 500～600 DEG C and be incubated 1 hour～2 hours, then be warming up to 1000 with the heating rate of 100 DEG C/h
～1100 DEG C, then it is warming up to 1350～1450 DEG C with the heating rate of 30～60 DEG C/h and is incubated 0.5～2 hour, then,
It is cooled to 1300～1400 DEG C and is incubated 20～60 hours, last Temperature fall.
The aluminium oxide ceramics that preparation method according to above-mentioned aluminium oxide ceramics prepares, described aluminium oxide ceramics average
Crystallite dimension is less than 100 nanometers.
A kind of plasma etch apparatus, containing above-mentioned aluminium oxide ceramics.
The preparation method of above-mentioned aluminium oxide ceramics is by the nano alumina powder using particle diameter to be 5～40 nanometers, and passes through
The inhibiting grain growth agent powder coordinating particle diameter to be 5～50 nanometers, by the method using above-mentioned gel injection-moulding, it is thus achieved that consistency is high
Biscuit, and by the sintering process of separate procedure, be effectively improved the consistency of pottery, prevent the abnormal growth of crystal grain,
Average grain size is made to be less than 100 nanometers；Reduce the addition of sintering aid so that pottery has higher purity simultaneously.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation method of the aluminium oxide ceramics of an embodiment.
Detailed description of the invention
For the ease of understanding the present invention, below with reference to relevant drawings, the present invention is described more fully.In accompanying 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.On the contrary, providing the purpose of these embodiments is to make the understanding to the disclosure more saturating
Thorough comprehensively.
Unless otherwise defined, all of technology used herein and scientific terminology and the technical field belonging to the present invention
The implication that technical staff is generally understood that is identical.The term used the most in the description of the invention is intended merely to describe tool
The purpose of the embodiment of body, it is not intended that in limiting the present invention.Term as used herein " and/or " include one or more phase
Arbitrary and all of combination of the Listed Items closed.
As it is shown in figure 1, the preparation method of the aluminium oxide ceramics of an embodiment, comprise the steps:
Step S110: add water mixing by organic monomer, cross-linking agent and dispersant, and regulate pH value to 9～10, obtain prewired
Liquid.
Wherein, organic monomer is acrylamide, Methacrylamide or n-methylolacrylamide；Cross-linking agent is that N, N'-are sub-
Bisacrylamide；Dispersant one in ammonium polyacrylate, ammonium citrate and Polyethylene Glycol.It is appreciated that at it
In its embodiment, cross-linking agent can also be poly-(ethylene glycol) methacrylate.
Wherein, in pre-mixing liquor, the weight/mass percentage composition of organic monomer is 10～20%, the weight/mass percentage composition of dispersant
Being 2～5%, organic monomer is 10:1～40:1 with the mass ratio of cross-linking agent.
Wherein, regulation pH value is ammonia to 9～10 reagent used.
Step S120: nano alumina powder and inhibiting grain growth agent powder are joined in pre-mixing liquor, blended, consolidate
The volumn concentration of phase be 35～45%, viscosity is less than the ceramic size of 1Pa s.
Wherein, nano alumina powder particle diameter (D50) is 5～40 nanometers.I.e. nano alumina powder particle diameter is that 5～40 nanometers are
50%.
Wherein, the particle diameter of inhibiting grain growth agent powder is 5～50 nanometers；And inhibiting grain growth agent powder and nano aluminium oxide
The mass ratio of powder is 0.5:100～1:100.Inhibiting grain growth agent powder is selected from magnesia powder and yttrium oxide powder at least
A kind of.
Wherein, the blend step after nano alumina powder and inhibiting grain growth agent powder being joined in pre-mixing liquor: ball milling
Mix 5～20 hours.
Step S130: add catalyst and initiator in ceramic size, through gelation, obtain wet base.
Wherein, initiator is Ammonium persulfate.；Initiator is 0.1:100～2:100 with the mass ratio of organic monomer.
Wherein, catalyst is N, N, N', N'-tetramethylethylenediamine；Catalyst is 0.1:100 with the mass ratio of organic monomer
～2:100.
Wherein, before ceramic size adds the step of catalyst and initiator, also include ceramic size evacuation
The step of degasification.Concrete, by ceramic size evacuation degasification 10～30 minutes.
Step S140: wet base is dried, more sintered, obtain aluminium oxide ceramics.
Wherein, the step being dried by wet base is: be dried at room temperature by wet base 1～5 day, then in 90～100 DEG C of insulations
10～20 hours, to remove the moisture in base that dehumidifies as much as possible.
Wherein, the step of sintering is: is warming up to 500～600 DEG C with the heating rate of 30～60 DEG C/h and is incubated 1 hour
～2 hours, then it is warming up to 1000～1100 DEG C with the heating rate of 100 DEG C/h, then with the intensification of 30～60 DEG C/h
Ramp is incubated 0.5～2 hour to 1350～1450 DEG C, then, is cooled to 1300 DEG C～1400 DEG C and is incubated 20～60 hours,
Last Temperature fall.Being warming up to 500～600 DEG C of insulations with the heating rate of 30～60 DEG C/h 1～2 hour is to remove
Organic substance.The relative density making base substrate in 0.5～2 hour 1350～1450 DEG C of insulations reaches 65～75%, and is cooled to
1300～1400 DEG C of insulations were obtained in that final fine and close aluminium oxide ceramics after 20～60 hours.Nano ceramics is to be difficult to sintering
, during high temperature sintering promotes densification, the fast growth of the crystal grain that invariably accompanies.Promote densification and suppression crystal grain
Growing up is the principal contradiction in nano ceramics technique, the most first reaches a high temperature and makes pottery shrink initial densification, the soonest
Speed is cooled to certain temperature, allows pottery that densification occurs on the premise of avoiding excessive grain to grow up, it is thus achieved that ultra-fine grain pottery.
The preparation method of above-mentioned aluminium oxide ceramics obtains the aluminium oxide ceramics of densification, and average grain size is less than 100 nanometers.
The preparation method of above-mentioned aluminium oxide ceramics is by the nano alumina powder using particle diameter to be 5～40 nanometers, and passes through
The inhibiting grain growth agent powder coordinating particle diameter to be 5～50 nanometers, by the method using above-mentioned gel injection-moulding, it is thus achieved that consistency is high
Biscuit, and by the sintering process of separate procedure, be effectively improved the consistency of pottery, prevent the abnormal growth of crystal grain,
So that the average grain size of aluminium oxide ceramics is less than 100 nanometers；Reduce the addition of sintering aid so that pottery tool simultaneously
There is higher purity.
The aluminium oxide ceramics that preparation method according to above-mentioned aluminium oxide ceramics prepares, the particle diameter of this aluminium oxide ceramics is little
In 100 nanometers, this aluminium oxide ceramics has aplitic texture, so that it has preferable anti-plasma corrosive nature.
Above-mentioned aluminium oxide ceramics can be applicable in plasma etch apparatus.
It is below specific embodiment part:
Embodiment 1
The preparation process of the aluminium oxide ceramics of the present embodiment is as follows:
(1) by acrylamide, N, N'-methylene-bisacrylamide and ammonium polyacrylate add deionized water stirring mixing, make
Regulating to pH value to 9 with ammonia, obtain pre-mixing liquor, wherein, in pre-mixing liquor, the weight/mass percentage composition of acrylamide is 15%,
The weight/mass percentage composition of ammonium polyacrylate is 3%, acrylamide and N, and the mass ratio of N'-methylene-bisacrylamide is 25:1.
(2) nano alumina powder and yttrium oxide powder are joined in pre-mixing liquor, mix 15 hours through ball milling, consolidate
The volumn concentration of phase is 40%, viscosity less than the ceramic size of 1Pa s, wherein, the particle diameter of nano alumina powder be 30～
40 nanometers, the particle diameter of yttrium oxide powder be the ratio of 5～10 nanometers, yttrium oxide and nano alumina powder be 0.8:100.
(3) by ceramic size evacuation degasification 20 minutes, then adding weight/mass percentage composition in ceramic size is 50%
N, the aqueous solution of N, N', N'-tetramethylethylenediamine and weight/mass percentage composition are the Ammonium persulfate. of 10%, inject in mould, solidifying
Gel 15 minutes, obtains wet base after demoulding.Wherein, N, N, N', N'-tetramethylethylenediamine is 1 with the mass ratio of acrylamide:
100；Ammonium persulfate. is 1:100 with the mass ratio of acrylamide.
(4) wet base is dried in the shade 3 days at room temperature, be incubated 15 hours in 95 DEG C the most in an oven, then in high temperature furnace
It is warming up to 600 DEG C with the heating rate of 45 DEG C/h and is incubated 1.5 hours, then be warming up to the heating rate of 100 DEG C/h
1100 DEG C, being then warming up to 1400 DEG C with the heating rate of 60 DEG C/h and be incubated 0.5 hour, then, furnace cooling is cooled to
1350 DEG C are incubated 20 hours, and last Temperature fall obtains aluminium oxide ceramics.
The detection method of the average crystal grain of the aluminium oxide ceramics of the present embodiment is as follows: aluminium oxide ceramics is carried out XRD test,
Average grain size is estimated with following Debye Scherrer formula (Debye-Scherrer).Wherein, D=K γ/(B cos θ), D is
Crystal grain is perpendicular to the average thickness (nm) of crystal plane direction；B is actual measurement sample diffraction peak width degree；θ is the angle of diffraction；γ is that X penetrates
Line wavelength, for 0.154056nm；K is Scherrer constant, if B is the halfwidth of diffraction maximum, then K=0.89；If B is diffraction maximum
Integration height width, then K=1.
The method of testing of the anti-plasma corrosive nature of the aluminium oxide ceramics of the present embodiment is as follows:
Aluminium oxide ceramics is cut into a size of 30mm × 30mm × 5mm, surface grinding is polished to roughness Ra≤0.5
μm, then covers polished surface peripheral position with Kapton Tape and reserves the exposed region of 20mm × 20mm at center.Make
With inductively coupled plasma etching system (Inductively Coupled Plasma Etching System, Germany
SENTECH, model SI 500) at CF4And O2Mixed gas plasma is irradiated process.By using DektakXT to visit
The shoulder height that stylus surface contourograph measurement is blanked and is not blanked between region is to determine corrosion depth, according to etching
Time Calculation goes out etch rate.Wherein, plasma exposure condition: etching gas is CF4(0.04L/min)+O2(0.01L/
Min), chamber pressure 5Pa, plasma power 100W.
The consistency of the aluminium oxide ceramics of the aluminium oxide ceramics of the present embodiment, particle diameter and etch rate are shown in Table 1.
Embodiment 2
The preparation process of the aluminium oxide ceramics of the present embodiment is as follows:
(1) by Methacrylamide, N, N'-methylene-bisacrylamide and ammonium citrate add deionized water stirring mixing,
Use ammonia to regulate to pH value to 10, obtain pre-mixing liquor, wherein, in pre-mixing liquor, the weight/mass percentage composition of Methacrylamide
Being 10%, the weight/mass percentage composition of ammonium citrate is 2%, Methacrylamide amine and N, the matter of N'-methylene-bisacrylamide
Amount ratio is 40:1.
(2) nano alumina powder and magnesia powder are joined in pre-mixing liquor, mix 5 hours through ball milling, obtain solid phase
Volumn concentration is 35%, viscosity less than the ceramic size of 1Pa s, wherein, the particle diameter of nano alumina powder is 20～30 to receive
Rice, the particle diameter of magnesium oxide is 5～50 nanometers, and magnesium oxide is 0.5:100 with the mass ratio of nano alumina powder.
(3) by ceramic size evacuation degasification 10 minutes, then adding weight/mass percentage composition in ceramic size is 50%
N, the aqueous solution of N, N', N'-tetramethylethylenediamine and weight/mass percentage composition are the Ammonium persulfate. of 10%, inject in mould, solidifying
Gel 20 minutes, obtains wet base after demoulding.Wherein, N, N, N', N'-tetramethylethylenediamine with the mass ratio of Methacrylamide is
0.1:100；Ammonium persulfate. is 0.1:100 with the mass ratio of Methacrylamide.
(4) wet base is dried in the shade 1 day at room temperature, be incubated 20 hours in 90 DEG C the most in an oven, then in high temperature furnace
It is warming up to 500 DEG C with the heating rate of 30 DEG C/h and is incubated 1 hour, then be warming up to 1000 with the heating rate of 100 DEG C/h
DEG C, then it is warming up to 1450 DEG C with the heating rate of 60 DEG C/h and is incubated 1 hour, then, furnace cooling is cooled to 1400 DEG C of guarantors
Temperature 60 hours, last Temperature fall, obtain aluminium oxide ceramics.
Use the identical method of testing of embodiment 1 obtain the consistency of aluminium oxide ceramics of the present embodiment, average crystal grain and
Etch rate is shown in Table 1.
Embodiment 3
The preparation process of the aluminium oxide ceramics of the present embodiment is as follows:
(1) by n-methylolacrylamide, N, it is mixed that N'-methylene-bisacrylamide and Polyethylene Glycol add deionized water stirring
Close, use ammonia to regulate to pH value to 10, obtain pre-mixing liquor, wherein, in pre-mixing liquor, the percent mass of n-methylolacrylamide
Content is 20%, and the percentage composition of Polyethylene Glycol is 5%, n-methylolacrylamide and N, the matter of N'-methylene-bisacrylamide
Amount ratio is 10:1.
(2) nano alumina powder, magnesia powder and yttrium oxide powder are joined in pre-mixing liquor, mix 20 through ball milling little
Time, the volumn concentration obtaining solid phase is 45%, the viscosity ceramic size less than 1Pa s, wherein, and nano alumina powder
Particle diameter is 5～40 nanometers, and the particle diameter of magnesia powder and yttrium oxide powder is 20～40 nanometers, and magnesia powder and three aoxidizes
The quality sum of two yttrium powder is 1:100 with the ratio of the quality of nano alumina powder.
(3) by ceramic size evacuation degasification 30 minutes, then adding weight/mass percentage composition in ceramic size is 50%
N, the aqueous solution of N, N', N'-tetramethylethylenediamine and weight/mass percentage composition are the Ammonium persulfate. of 10%, inject in mould, solidifying
Gel 10 minutes, obtains wet base after demoulding.Wherein, N, N, N', N'-tetramethylethylenediamine and the mass ratio of n-methylolacrylamide
For 2:100；Ammonium persulfate. is 2:100 with the mass ratio of n-methylolacrylamide.
(4) wet base is dried in the shade 5 days at room temperature, be incubated 10 hours in 100 DEG C the most in an oven, then in high temperature furnace
It is warming up to 600 DEG C with the heating rate of 60 DEG C/h and is incubated 1 hour, then be warming up to 1100 with the heating rate of 100 DEG C/h
DEG C, then it is warming up to 1350 DEG C with the heating rate of 60 DEG C/h and is incubated 1 hour, then, furnace cooling is cooled to 1330 DEG C of guarantors
Temperature 50 hours, last Temperature fall, obtain aluminium oxide ceramics.
Use the identical method of testing of embodiment 1 obtain the consistency of aluminium oxide ceramics of the present embodiment, average crystal grain and
Etch rate is shown in Table 1.
Comparative example 1
The preparation process of the aluminium oxide ceramics of the present embodiment is as follows:
(1) by Methacrylamide, N, N'-methylene-bisacrylamide and ammonium citrate add deionized water stirring mixing,
Use ammonia to regulate to pH value to 10, obtain pre-mixing liquor, wherein, in pre-mixing liquor, the weight/mass percentage composition of Methacrylamide
Being 10%, the weight/mass percentage composition of ammonium citrate is 2%, Methacrylamide amine and N, the matter of N'-methylene-bisacrylamide
Amount ratio is 40:1.
(2) nano alumina powder and magnesium oxide are joined in pre-mixing liquor, mix 5 hours through ball milling, obtain the body of solid phase
Long-pending percentage composition is 50%, viscosity less than the ceramic size of 1Pa s, wherein, the particle diameter of nano alumina powder is 0.5～1 micro-
Rice, the particle diameter of yttrium oxide powder is 5～10 nanometers, and magnesium oxide is 0.5:100 with the mass ratio of nano alumina powder.
(3) by ceramic size evacuation degasification 10 minutes, then adding weight/mass percentage composition in ceramic size is 50%
N, the aqueous solution of N, N', N'-tetramethylethylenediamine and weight/mass percentage composition are the Ammonium persulfate. of 10%, inject in mould, solidifying
Gel 20 minutes, obtains wet base after demoulding.Wherein, N, N, N', N'-tetramethylethylenediamine with the mass ratio of Methacrylamide is
0.1:100；Ammonium persulfate. is 0.1:100 with the mass ratio of Methacrylamide.
(4) wet base is dried in the shade 1 day at room temperature, be incubated 20 hours in 90 DEG C the most in an oven, then in high temperature furnace
It is warming up to 500 DEG C with the heating rate of 30 DEG C/h and is incubated 1 hour, then be warming up to 1000 with the heating rate of 100 DEG C/h
DEG C, then it is warming up to 1650 DEG C with the heating rate of 60 DEG C/h and is incubated 2 hours, Temperature fall, obtain aluminium oxide ceramics.
The method of testing using embodiment 1 identical obtains the consistency of aluminium oxide ceramics, average crystal grain and the quarter of comparative example 1
Erosion speed is shown in Table 1.
Comparative example 2
The preparation process of the aluminium oxide ceramics of comparative example 2 is as follows:
By alumina powder jointed for micron order that particle diameter is 5nm and magnesium oxide according to 100:0.5 mixing wet ball grinding, 90 DEG C of bakings
Dry, then isostatic pressing, 1450 DEG C of insulation 5h, obtain aluminium oxide ceramics.
The method of testing using embodiment 1 identical obtains the consistency of aluminium oxide ceramics, average crystal grain and the quarter of comparative example 1
Erosion speed is shown in Table 1.
Table 1 is embodiment 1～3 and the consistency, flat of aluminium oxide ceramics of aluminium oxide ceramics of comparative example 1 and comparative example 2
All crystal grain and etch rates.
Table 1
From table 1 it follows that the most at least the 99.5% of the aluminium oxide ceramics of embodiment 1～3, average crystal grain particle diameter
Maximum only 96 nanometers, the etch rate of the aluminium oxide ceramics of embodiment 1～3 at most only 0.7 nm/minute, and comparative example 1
The etch rate of aluminium oxide ceramics be 3.9 nm/minute, the etch rate of the aluminium oxide ceramics of comparative example 2 be 12.3 nanometers/
Minute, the most significantly larger than embodiment 1 and embodiment 3, it is clear that it is rotten that the aluminium oxide ceramics of the application has more preferable anti-plasma
Erosion performance.
Each technical characteristic of embodiment described above can combine arbitrarily, for making description succinct, not to above-mentioned reality
The all possible combination of each technical characteristic executed in example is all described, but, as long as the combination of these technical characteristics is not deposited
In contradiction, all it is considered to be the scope that this specification is recorded.
Embodiment described above only have expressed the several embodiments of the present invention, and it describes more concrete and detailed, but also
Can not therefore be construed as limiting the scope of the patent.It should be pointed out that, come for those of ordinary skill in the art
Saying, without departing from the inventive concept of the premise, it is also possible to make some deformation and improvement, these broadly fall into the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. the preparation method of an aluminium oxide ceramics, it is characterised in that comprise the steps:
Add water mixing by organic monomer, cross-linking agent and dispersant, and regulates pH value to 9～10, obtains pre-mixing liquor；
Nano alumina powder and inhibiting grain growth agent powder are joined in described pre-mixing liquor, blended, obtain the volume of solid phase
Percentage composition be 35～45%, viscosity less than the ceramic size of 1Pa s, wherein, the particle diameter of described nano alumina powder be 5～
40 nanometers, the particle diameter of described inhibiting grain growth agent powder is 5～50 nanometers；
In described ceramic size, add catalyst and initiator, through gelation, obtain wet base；
Described wet base is dried, more sintered, obtain aluminium oxide ceramics.
The preparation method of aluminium oxide ceramics the most according to claim 1, it is characterised in that described organic monomer is acryloyl
Amine, Methacrylamide or n-methylolacrylamide；Described cross-linking agent is N, N'-methylene-bisacrylamide；Described dispersant
One in ammonium polyacrylate, ammonium citrate and Polyethylene Glycol.
The preparation method of aluminium oxide ceramics the most according to claim 1, it is characterised in that in described pre-mixing liquor, described
The weight/mass percentage composition of organic monomer is 10～20%, and the weight/mass percentage composition of described dispersant is 2～5%, described organic list
Body is 10:1～40:1 with the mass ratio of described cross-linking agent.
The preparation method of aluminium oxide ceramics the most according to claim 1, it is characterised in that described inhibiting grain growth agent powder
It is 0.5:100～1:100 with the mass ratio of described nano alumina powder；Described inhibiting grain growth agent powder selected from magnesia powder and
At least one in yttrium oxide powder.
The preparation method of aluminium oxide ceramics the most according to claim 1, it is characterised in that described initiator is persulfuric acid
Ammonium, described catalyst is N, N, N', N'-tetramethylethylenediamine.
The preparation method of aluminium oxide ceramics the most according to claim 1, it is characterised in that add in described ceramic size
Before the step of described catalyst and described initiator, also include the step of described ceramic size evacuation de-bubble.
The preparation method of aluminium oxide ceramics the most according to claim 1, it is characterised in that the step that described wet base is dried
For: described wet base is dried at room temperature 1～5 day, is then incubated 10～20 hours in 90～100 DEG C.
The preparation method of aluminium oxide ceramics the most according to claim 1, it is characterised in that the step of described sintering is: with
The heating rate of 30～60 DEG C/h is warming up to 500～600 DEG C and is incubated 1 hour～2 hours, then the intensification with 100 DEG C/h
Ramp, to 1000～1100 DEG C, is then warming up to 1350～1450 DEG C of insulations 0.5 with the heating rate of 30～60 DEG C/h
～2 hours, then, it is cooled to 1300～1400 DEG C and is incubated 20～60 hours, last Temperature fall.
9. the aluminium oxide ceramics obtained according to the preparation method of the aluminium oxide ceramics described in claim 1～8 any one, it is special
Levying and be, the average grain size of described aluminium oxide ceramics is less than 100 nanometers.
10. a plasma etch apparatus, it is characterised in that containing the aluminium oxide ceramics described in claim 9.
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