CN1207247C - Prepn process of aluminium nitride ceramic substrate - Google Patents
Prepn process of aluminium nitride ceramic substrate Download PDFInfo
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Abstract
The present invention relates to the improvement of a preparation method for an aluminum nitride ceramic substrate, which belongs to the field of an inorganic non-metal material. The present invention uses aluminum oxide, and hydrophilic graphite or carbon black as major raw materials to prepare the aluminum nitride ceramic substrate and has the processing steps: material compounding, blank molding, blank drying, sand spraying and laminating, carbon thermal reduction and nitriding reaction, carbon residue burning, polishing for eliminating isolating sand and flattening. The present invention has the advantages that the sources of raw materials are sufficient, cost is reduced to 1/70 to 1/80 of original cost, and simultaneously, the problem of environmental pollution dose not exist.
Description
Technical field: the invention belongs to field of inorganic nonmetallic material, relate to improvement to the aluminium nitride ceramic substrate preparation method.
Background technology: traditional aluminium nitride ceramics mainly is that to adopt aluminum nitride powder be raw material, and forming technique mainly contains dry pressing, hot isostatic pressing method, rolls embrane method, organic casting method etc.Sintering densification mainly adopts two kinds of pressure sintering, sintering processs.Since the aluminium nitride powder complicated process of preparation, equipment requirements condition height, and so cause aluminium nitride powder to cost an arm and a leg, the existing market price is about 450 yuan/kg.And the sintering process of aluminium nitride is relatively harsher, and sintering or hot pressed sintering temperature are often up to more than 1800 ℃, because the prices of raw and semifnished materials are expensive and the factor of this two aspect of complex process, causes the preparation difficulty of aluminium nitride ceramics material.In addition, aluminium nitride powder is hydrolysis very easily, so aluminium nitride ceramics base sheet can not prepare with aqueous slurries, when utilizing organic slip to prepare, because the organic solvent that is adopted has very strong volatility, environment and human body is caused detrimentally affect, has problem of environmental pollution.
Summary of the invention: technical problem to be solved by this invention is, at traditional aluminium nitride ceramics material cost height, energy consumption is big, problems such as efficient is low, proposing a kind of is raw material with cheap aluminum oxide powder and graphite or carbon black, the method for preparing aluminium nitride ceramic substrate, present method can be utilized and roll modulus method, gel casting (Gel-Casting), multiple forming methods such as organic curtain coating, water-based tape casting are prepared, have the base substrate of machinability energy after acquisition dehydrates, thereby greatly reduce the preparation cost of aluminium nitride ceramic substrate.
Technical scheme of the present invention is: a kind of method for preparing aluminium nitride ceramic substrate is characterized in that utilize aluminum oxide and wetting ability graphite or carbon black to prepare aluminium nitride ceramic substrate for main raw material, its processing step is as follows:
1.1, batching, according to the composition requirement of prepared ceramic green sheet, accurate weighing aluminum oxide powder powder stock; Take by weighing reaction promoter, it can be CaF
2, Y
2O
3, YF
6, CaO, CaCO
3, BN one of them or the wherein combination of several materials, promoter addition is 0.5～5wt% of alumina powder weight; Take by weighing wetting ability graphite or carbon black powder, its add-on is the 10wt%～25wt% of alumina powder,
1.2, the moulding of base sheet, the moulding of base sheet can be adopted one of following method: gel is cast type, injection moulding, rolling formation, organic flow casting molding, aqueous tape casting forming,
1.3, base sheet drying, after slurry gelization was finished, disengageding mould was positioned over base substrate on the gas-pervious mesh screen or on the smooth plasterboard it is dehydrated, drying mode can adopt seasoning, blowing drying or heat drying,
1.4, the lamination that sands, onesize ceramic green sheet is stacked together, 1～15 every pile, spill one deck corundum sand between sheet and the sheet equably, snarl with adhesive tape then,
1.5, carbothermal reduction-nitridation reaction, the ceramic green sheet that has spread sand is placed on N
2Carry out carbothermic reduction reaction in the atmosphere furnace, wherein, N
2Flow is 1～5L/min, and temperature rise rate is controlled at 5～20 ℃, at first is raised to 500～700 ℃ of insulation 0.5～5h, is warmed up to 1600～1800 ℃ of insulation 2～8h then, come out of the stove when being cooled at last not be higher than 200 ℃,
1.6, the carbon residue burn off, the porcelain body of coming out of the stove in the nitrogen furnace is placed on carries out the carbon residue burn off in the air furnace and handle, technological temperature is 600～800 ℃, soaking time 2～10h,
1.7, rubbing down removes parting sand, will finish ceramic plate behind the carbon residue burn off and in water, carry out rubbing down and handle, with the isolation sand on removing ceramics surface,
1.8, cover flat the processing, ceramics covers flat the processing under nitrogen atmosphere the most at last, guarantees the planeness of substrate.Wherein, cover to put down being lower than under 200～300 ℃ of the sintering temperatures and carry out, covering at ordinary times, soaking time is 2～4h.
The invention has the beneficial effects as follows, solved the low-cost technology of preparing of aluminium nitride ceramic substrate, and proposed a whole set of technical scheme, make it to be adapted to the suitability for industrialized production requirement.Its advantage mainly shows as:
The first, compare with the preparation method of general both at home and abroad at present aluminium nitride ceramics, replace aluminum nitride powder as raw material with alumina powder and wetting ability graphite or carbon black, the starting material source is sufficient, and its cost reduces significantly, be reduced to originally 1/70～1/80, also do not have problem of environmental pollution simultaneously.
The second, this technology can be coagulated method, organic casting method, water base casting process by means of water base notes, be rolled traditional technology methods such as modulus method and prepare ceramic body, the tooling comparative maturity is reliable, easily manufactured, the production efficiency height selects suitable body preparation method can produce the ceramic body of different shape easily and flexibly.
Three, this process using aluminum oxide powder and wetting ability graphite or carbon black and auxiliary agent are as the starting material of aluminium nitride preparation, in the ceramic body of preparing, mix between the each component like this, help reacting fully carrying out of transformation, also can guarantee the homogeneity of last porcelain body composition and tissue.
Four, the present invention selects suitable sintering agent for use, as CaF
2, Y
2O
3, YF
6, CaCO
3, BN etc. one or more, can make the formation temperature of final aluminium nitride reduce about 100～200 ℃ than traditional technology, energy conservation and consumption reduction effects is very remarkable.And the porcelain body relative density of preparing is not prone to cracking phenomena up to 99.5%, thermal conductivity up to 60～150W/mK about.
Description of drawings: Fig. 1 is the process flow sheet of preparation aluminium nitride ceramic substrate of the present invention.
Embodiment: the present invention is described in further details below in conjunction with accompanying drawing.Fig. 1 has provided with alumina powder and wetting ability graphite or carbon black, and to be raw material prepare the complete process flow of aluminium nitride ceramic substrate by the carbothermal reduction-nitridation method, and technical process of the present invention begins behind the final sintering till the carbon residue burn off from batching.
One, batching.According to the composition requirement of required stupalith, accurate weighing ceramic powder, graphite or carbon black powder and auxiliary agent powder.The auxiliary agent that is adopted has: (1) CaF
2, it act as the attenuating reaction activity, impels reaction to carry out; (2) Y
2O
3, it act as the formation cocrystalization compound, impels reaction to carry out; (3) CaO is (with CaCO
3Form is introduced), reduce reaction activity, advance reaction to carry out; (4) CaF
2-Y
2O
3Two component system; (5) CaF
2-YF
6Two component system; (6) CaF
2-Y
2O
3-BN three component system.
Two, base sheet moulding.The moulding of base sheet can adopt gel to cast moulding ways such as type (Gel-Casting), injection moulding, rolling formation, organic curtain coating, aqueous tape casting forming.(application number is: 01104148 as gel casting patent Chinese patent; ) and United States Patent (USP) (patent No.: 6136241 and 5788891), water-based tape casting patent (patent No. is CN1263812 and CN1257852), organic curtain coating patent (patent No. is US Patent); Peng Yi [ceramic engineering, 2000,02], Lang Jing [Wuhan Transportation University journal, 1997,06] and Jia Yuanmin [casting, 1997,07] have studied hot die-casting molding technology respectively; Wu Yin [Journal of Inorganic Materials, 1996,04] and Li Guorong [silicate journal, 1999,05] have been studied organic curtain coating forming technique respectively.
For example, when adopting gel to cast the type method, its main processing step is as follows:
Gel is cast type technology, and detailed content can (application number be: 01104148) referring to patent documentation.
A, batching.
According to the composition requirement of prepared ceramic green sheet, accurate weighing aluminum oxide powder powder stock; Take by weighing reaction promoter, it can be CaF
2, Y
2O
3, YF
6, CaO, CaCO
3, BN one of them or the wherein combination of several materials, promoter addition is 0.5～5wt% of alumina powder weight; Take by weighing wetting ability graphite or carbon black powder, its add-on is the 10wt%～25wt% of alumina powder.
Weighing deionized water or distilled water to scale; Take by weighing dispersion agent, it is one of following material: polyacrylate, poly-methyl acrylate, carbonyl hydrochlorate, Citrate trianion, its add-on are 0.5～2.0% of ceramic powder weight; Take by weighing the hydrophilic graphite ink powder, its add-on is the 10wt%～25wt% of ceramic raw material; Take by weighing organic monomer and linking agent, organic monomer is water soluble propene's acid amides or Methacrylamide, linking agent is methylene-bisacrylamide or many ethyleneglycol dimethacrylates, the ratio of organic monomer and linking agent can be chosen between 10: 1～30: 1, and total add-on is 10～30% of a water weight.
B, mixing and ball milling.
With above-mentioned ceramic powder, Graphite Powder 99, deionized water or distilled water, dispersion agent, softening agent, suspension agent, organic monomer and linking agent are put into fully ball milling of ball mill, form ceramic slurry, and the ball milling time is 10～30h, and ratio of grinding media to material is 1: 1～2: 1;
C, cast molding.
After the ball milling discharging, at first want degasification, ceramic slurry is carried out vacuum stirring or vibration degasification, add the defoamer of slip total amount 0.5～2%; Add initiator then, add the initiator ammonium persulfate aqueous solution in the ceramic slurry after the vacuum stirring degasification, stir, the add-on of initiator is 0.2～0.6% of an organic monomer weight; At last ceramic slurry is injected the mould gel, can adopt following two kinds of methods one of them:
C-1, add the catalyzer Tetramethyl Ethylene Diamine in ceramic slurry, treat its natural gelation in the back cast progressive die tool that stirs, the add-on of catalyzer is 0.05～0.5% of an organic monomer weight.
C-2 is heated to 40～80 ℃ and makes ceramic slurry gelization after ceramic slurry is poured into a mould the progressive die tool.
For another example, when adopting method for forming water-base casting, its main processing step is as follows:
Aqueous tape casting forming technology, detailed content can be referring to patent CN1263812 and CN1257852.
Three, base sheet drying.After slurry gelization is finished, disengageding mould is positioned over base substrate on the gas-pervious mesh screen or on the smooth plasterboard it is dehydrated, and drying mode can adopt seasoning, blowing drying or heat drying, but require the dehydration of full wafer even green body, avoid base substrate generation gross distortion.Can obtain having certain snappiness after base substrate dehydrates, any surface finish is smooth, can satisfy the ceramic body of mechanical workout.
Four, the lamination that sands.Onesize ceramic green sheet is stacked together, 1～15 every pile, spill one deck corundum sand between sheet and the sheet equably, snarl with adhesive tape then.
Five, carbothermal reduction-nitridation is handled.Be placed on N with having spread husky base sheet
2Heat-treat in the atmosphere furnace, employed stove can be atmosphere sintering furnaces such as box-type furnace, kind cover stove, tunnel furnace.N
2Flow is 1～5L/min, and temperature rise rate is controlled at 5～20 ℃, at first is raised to 500～700 ℃, and insulation 0.5～5h is warmed up to 1600～1800 ℃ then, and insulation 2～8h comes out of the stove when being cooled to then not be higher than 200 ℃.
Six, carbon residue burn off.The porcelain body of coming out of the stove in the nitrogen furnace is placed on carries out the carbon residue burn off in the air furnace and handle, technological temperature is 600～800 ℃, time 2～10h.
Seven, rubbing down is removed parting sand.To finish ceramic plate behind the carbon residue burn off and in water, carry out rubbing down and handle, to remove the isolation sand on ceramics surface.
Eight, cover flat the processing.Ceramics covers flat the processing under nitrogen atmosphere the most at last, guarantees the planeness of substrate.Wherein, cover to put down being lower than under 200～300 ℃ of the sintering temperatures and carry out, covering at ordinary times, soaking time is 2～4h.
The embodiment of aluminium nitride electronic ceramic substrate preparation.
Table 1 and table 2 provide the processing parameter of 300 specific embodiments.Table 1 is made up of table 1-1～table 1-5, and table 2 also is made up of table 2-1～table 2-5, and table 2-1～table 2-5 is respectively the continuous table of table 1-1～table 1-5.Wherein, starting material adopt purity greater than 99.5%, α-Al of median size 2.84 μ m
2O
3Powder, median size are wetting ability graphite or the carbon black powder of 2.5 μ m.Above-mentioned base sheet is stacked to 15 at most, and density can reach 3.26～3.29g/cm behind the sintering
3Thermal conductivity reaches 60～150W/mK (25 ℃).
Table 1-1 is with the embodiment processing parameter (continued) of Calcium Fluoride (Fluorspan) as additive
| The embodiment sequence number | Prescription (wt%) | Molding mode | Base sheet drying | |
| Al 2O 3: hydrophilic graphite or carbon black (weight ratio | Auxiliary agent content (wt%) | |||
| 1 | 90∶10 | CaF 2，0.5％ | The gel casting | 80 ℃ of oven dry |
| 2 | 90∶10 | CaF 2，0.5％ | Water-based tape casting | 80 ℃ of oven dry |
| 3 | 90∶10 | CaF 2，0.5％ | Roll film | 80 ℃ of oven dry |
| 4 | 90∶10 | CaF 2，0.5％ | Injection moulding | 80 ℃ of oven dry |
| 5 | 90∶10 | CaF 2，0.5％ | Organic curtain coating | 80 ℃ of oven dry |
| 6 | 90∶10 | CaF 2，1.0％ | The gel casting | 80 ℃ of oven dry |
| 7 | 90∶10 | CaF 2，1.0％ | Water-based tape casting | 80 ℃ of oven dry |
| 8 | 90∶10 | CaF 2，1.0％ | Roll embrane method | 80 ℃ of oven dry |
| 9 | 90∶10 | CaF 2，1.0％ | Injection moulding | 80 ℃ of oven dry |
| 10 | 90∶10 | CaF 2，1.0％ | Organic curtain coating | 80 ℃ of oven dry |
| 11 | 90∶10 | CaF 2，2.0％ | The gel casting | 80 ℃ of oven dry |
| 12 | 90∶10 | CaF 2，2.0％ | Water-based tape casting | 80 ℃ of oven dry |
| 13 | 90∶10 | CaF 2，2.0％ | Roll embrane method | 80 ℃ of oven dry |
| 14 | 90∶10 | CaF 2，2.0％ | Injection moulding | 80 ℃ of oven dry |
| 15 | 90∶10 | CaF 2，2.0％ | Organic curtain coating | 80 ℃ of oven dry |
| 16 | 85∶15 | CaF 2，0.5％ | The gel casting | 80 ℃ of oven dry |
| 17 | 85∶15 | CaF 2，0.5％ | Water-based tape casting | 80 ℃ of oven dry |
| 18 | 85∶15 | CaF 2，0.5％ | Roll embrane method | 80 ℃ of oven dry |
| 19 | 85∶15 | CaF 2，0.5％ | Injection moulding | 80 ℃ of oven dry |
| 20 | 85∶15 | CaF 2，0.5％ | Organic curtain coating | 75 ℃ of oven dry |
| 21 | 85∶15 | CaF 2，1.0％ | The gel casting | 75 ℃ of oven dry |
| 22 | 85∶15 | CaF 2，1.0％ | Water-based tape casting | 75 ℃ of oven dry |
| 23 | 85∶15 | CaF 2，1.0％ | Roll embrane method | 75 ℃ of oven dry |
| 24 | 85∶15 | CaF 2，1.0％ | Injection moulding | 75 ℃ of oven dry |
| 25 | 85∶15 | CaF 2，1.0％ | Organic curtain coating | 75 ℃ of oven dry |
| 26 | 85∶15 | CaF 2，2.0％ | The gel casting | 75 ℃ of oven dry |
| 27 | 85∶15 | CaF 2，2.0％ | Water-based tape casting | 75 ℃ of oven dry |
| 28 | 85∶15 | CaF 2，2.0％ | Roll embrane method | 75 ℃ of oven dry |
| 29 | 85∶15 | CaF 2，2.0％ | Injection moulding | 70 ℃ of oven dry |
| 30 | 85∶15 | CaF 2，2.0％ | Organic curtain coating | 70 ℃ of oven dry |
| 31 | 80∶20 | CaF 2，0.5％ | The gel casting | 70 ℃ of oven dry |
| 32 | 80∶20 | CaF 2，0.5％ | Water-based tape casting | 70 ℃ of oven dry |
| 33 | 80∶20 | CaF 2，0.5％ | Roll embrane method | 70 ℃ of oven dry |
| 34 | 80∶20 | CaF 2，0.5％ | Injection moulding | 70 ℃ of oven dry |
| 35 | 80∶20 | CaF 2，0.5％ | Organic curtain coating | 70 ℃ of oven dry |
| 36 | 80∶20 | CaF 2，1.0％ | The gel casting | 70 ℃ of oven dry |
| 37 | 80∶20 | CaF 2，1.0％ | Water-based tape casting | 70 ℃ of oven dry |
| 38 | 80∶20 | CaF 2，1.0％ | Roll embrane method | 70 ℃ of oven dry |
| 39 | 80∶20 | CaF 2，1.0％ | Injection moulding | 70 ℃ of oven dry |
| 40 | 80∶20 | CaF 2，1.0％ | Organic curtain coating | 70 ℃ of oven dry |
| 41 | 80∶20 | CaF 2，2.0％ | The gel casting | 65 ℃ of oven dry |
| 42 | 80∶20 | CaF 2，2.0％ | Water-based tape casting | 65 ℃ of oven dry |
| 43 | 80∶20 | CaF 2，2.0％ | Roll embrane method | 65 ℃ of oven dry |
| 44 | 80∶20 | CaF 2，2.0％ | Injection moulding | 65 ℃ of oven dry |
| 45 | 80∶20 | CaF 2，2.0％ | Organic curtain coating | 65 ℃ of oven dry |
| 46 | 75∶25 | CaF 2，0.5％ | The gel casting | 65 ℃ of oven dry |
| 47 | 75∶25 | CaF 2，0.5％ | Water-based tape casting | 65 ℃ of oven dry |
| 48 | 75∶25 | CaF 2，0.5％ | Roll embrane method | 65 ℃ of oven dry |
| 49 | 75∶25 | CaF 2，0.5％ | Injection moulding | 65 ℃ of oven dry |
| 50 | 75∶25 | CaF 2，0.5％ | Organic curtain coating | 65 ℃ of oven dry |
| 51 | 75∶25 | CaF 2，1.0％ | The gel casting | 60 ℃ of oven dry |
| 52 | 75∶25 | CaF 2，1.0％ | Water-based tape casting | 60 ℃ of oven dry |
| 53 | 75∶25 | CaF 2，1.0％ | Roll embrane method | 60 ℃ of oven dry |
| 54 | 75∶25 | CaF 2，1.0％ | Injection moulding | 60 ℃ of oven dry |
| 55 | 75∶25 | CaF 2，1.0％ | Organic curtain coating | 60 ℃ of oven dry |
| 56 | 75∶25 | CaF 2，2.0％ | The gel casting | 60 ℃ of oven dry |
| 57 | 75∶25 | CaF 2，2.0％ | Water-based tape casting | 60 ℃ of oven dry |
| 58 | 75∶25 | CaF 2，2.0％ | Roll embrane method | 60 ℃ of oven dry |
| 59 | 75∶25 | CaF 2，2.0％ | Injection moulding | 60 ℃ of oven dry |
| 60 | 75∶25 | CaF 2，2.0％ | Organic curtain coating | 60 ℃ of oven dry |
Table 1-2 is with the embodiment processing parameter (continued) of yttrium oxide as additive
| The embodiment sequence number | Prescription (wt%) | Molding mode | Base sheet drying | |
| Al 2O 3: hydrophilic graphite or carbon black (weight ratio | Auxiliary agent content (wt%) | |||
| 61 | 90∶10 | Y 2O 3，0.5％ | The gel casting | 80 ℃ of oven dry |
| 62 | 90∶10 | Y 2O 3，0.5％ | Water-based tape casting | 80 ℃ of oven dry |
| 63 | 90∶10 | Y 2O 3，0.5％ | Roll embrane method | 80 ℃ of oven dry |
| 64 | 90∶10 | Y 2O 3，0.5％ | Injection moulding | 80 ℃ of oven dry |
| 65 | 90∶10 | Y 2O 3，0.5％ | Organic curtain coating | 80 ℃ of oven dry |
| 66 | 90∶10 | Y 2O 3，1.0％ | The gel casting | 80 ℃ of oven dry |
| 67 | 90∶10 | Y 2O 3，1.0％ | Water-based tape casting | 80 ℃ of oven dry |
| 68 | 90∶10 | Y 2O 3，1.0％ | Roll embrane method | 80 ℃ of oven dry |
| 69 | 90∶10 | Y 2O 3，1.0％ | Injection moulding | 80 ℃ of oven dry |
| 70 | 90∶10 | Y 2O 3，1.0％ | Organic curtain coating | 80 ℃ of oven dry |
| 71 | 90∶10 | Y 2O 3，2.0％ | The gel casting | 75 ℃ of oven dry |
| 72 | 90∶10 | Y 2O 3，2.0％ | Water-based tape casting | 75 ℃ of oven dry |
| 73 | 90∶10 | Y 2O 3，2.0％ | Roll embrane method | 75 ℃ of oven dry |
| 74 | 90∶10 | Y 2O 3，2.0％ | Injection moulding | 75 ℃ of oven dry |
| 75 | 90∶10 | Y 2O 3，2.0％ | Organic curtain coating | 75 ℃ of oven dry |
| 76 | 85∶15 | Y 2O 3，0.5％ | The gel casting | 75 ℃ of oven dry |
| 77 | 85∶15 | Y 2O 3，0.5％ | Water-based tape casting | 75 ℃ of oven dry |
| 78 | 85∶15 | Y 2O 3，0.5％ | Roll embrane method | 75 ℃ of oven dry |
| 79 | 85∶15 | Y 2O 3，0.5％ | Injection moulding | 75 ℃ of oven dry |
| 80 | 85∶15 | Y 2O 3，0.5％ | Organic curtain coating | 75 ℃ of oven dry |
| 81 | 85∶15 | Y 2O 3，1.0％ | The gel casting | 70 ℃ of oven dry |
| 82 | 85∶15 | Y 2O 3，1.0％ | Water-based tape casting | 70 ℃ of oven dry |
| 83 | 85∶15 | Y 2O 3，1.0％ | Roll embrane method | 70 ℃ of oven dry |
| 84 | 85∶15 | Y 2O 3，1.0％ | Injection moulding | 70 ℃ of oven dry |
| 85 | 85∶15 | Y 2O 3，1.0％ | Organic curtain coating | 70 ℃ of oven dry |
| 86 | 85∶15 | Y 2O 3，2.0％ | The gel casting | 70 ℃ of oven dry |
| 87 | 85∶15 | Y 2O 3，2.0％ | Water-based tape casting | 70 ℃ of oven dry |
| 88 | 85∶15 | Y 2O 3，2.0％ | Roll embrane method | 70 ℃ of oven dry |
| 89 | 85∶15 | Y 2O 3，2.0％ | Injection moulding | 70 ℃ of oven dry |
| 90 | 85∶15 | Y 2O 3，2.0％ | Organic curtain coating | 65 ℃ of oven dry |
| 91 | 80∶20 | Y 2O 3，0.5％ | The gel casting | 65 ℃ of oven dry |
| 92 | 80∶20 | Y 2O 3，0.5％ | Water-based tape casting | 65 ℃ of oven dry |
| 93 | 80∶20 | Y 2O 3，0.5％ | Roll embrane method | 65 ℃ of oven dry |
| 94 | 80∶20 | Y 2O 3，0.5％ | Injection moulding | 65 ℃ of oven dry |
| 95 | 80∶20 | Y 2O 3，0.5％ | Organic curtain coating | 65 ℃ of oven dry |
| 96 | 80∶20 | Y 2O 3，1.0％ | The gel casting | 65 ℃ of oven dry |
| 97 | 80∶20 | Y 2O 3，1.0％ | Water-based tape casting | 65 ℃ of oven dry |
| 98 | 80∶20 | Y 2O 3，1.0％ | Roll embrane method | 65 ℃ of oven dry |
| 99 | 80∶20 | Y 2O 3，1.0％ | Injection moulding | 65 ℃ of oven dry |
| 100 | 80∶20 | Y 2O 3，1.0％ | Organic curtain coating | 65 ℃ of oven dry |
| 101 | 80∶20 | Y 2O 3，2.0％ | The gel casting | 65 ℃ of oven dry |
| 102 | 80∶20 | Y 2O 3，2.0％ | Water-based tape casting | 65 ℃ of oven dry |
| 103 | 80∶20 | Y 2O 3，2.0％ | Roll embrane method | 65 ℃ of oven dry |
| 104 | 80∶20 | Y 2O 3，2.0％ | Injection moulding | 65 ℃ of oven dry |
| 105 | 80∶20 | Y 2O 3，2.0％ | Organic curtain coating | 60 ℃ of oven dry |
| 106 | 75∶25 | Y 2O 3，0.5％ | The gel casting | 60 ℃ of oven dry |
| 107 | 75∶25 | Y 2O 3，0.5％ | Water-based tape casting | 60 ℃ of oven dry |
| 108 | 75∶25 | Y 2O 3，0.5％ | Roll embrane method | 60 ℃ of oven dry |
| 109 | 75∶25 | Y 2O 3，0.5％ | Injection moulding | 60 ℃ of oven dry |
| 110 | 75∶25 | Y 2O 3，0.5％ | Organic curtain coating | 60 ℃ of oven dry |
| 111 | 75∶25 | Y 2O 3，1.0％ | The gel casting | 60 ℃ of oven dry |
| 112 | 75∶25 | Y 2O 3，1.0％ | Water-based tape casting | 60 ℃ of oven dry |
| 113 | 75∶25 | Y 2O 3，1.0％ | Roll embrane method | 60 ℃ of oven dry |
| 114 | 75∶25 | Y 2O 3，1.0％ | Injection moulding | 60 ℃ of oven dry |
| 115 | 75∶25 | Y 2O 3，1.0％ | Organic curtain coating | 60 ℃ of oven dry |
| 116 | 75∶25 | Y 2O 3，2.0％ | The gel casting | 60 ℃ of oven dry |
| 117 | 75∶25 | Y 2O 3，2.0％ | Water-based tape casting | 60 ℃ of oven dry |
| 118 | 75∶25 | Y 2O 3，2.0％ | Roll embrane method | 60 ℃ of oven dry |
| 119 | 75∶25 | Y 2O 3，2.0％ | Injection moulding | 60 ℃ of oven dry |
| 120 | 75∶25 | Y 2O 3，2.0％ | Organic curtain coating | 60 ℃ of oven dry |
Table 1-3 is with the embodiment processing parameter (continued) of Calcium Fluoride (Fluorspan)-yttrium oxide as additive
| The embodiment sequence number | Prescription (wt%) | Molding mode | Base sheet drying | |
| Al 2O 3: hydrophilic graphite or carbon black (weight ratio | Auxiliary agent content (wt%) | |||
| 121 | 90∶10 | CaF 2-Y 2O 3Respectively account for 0.5wt% | The gel casting | 80 ℃ of oven dry |
| 122 | 90∶10 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Water-based tape casting | 80 ℃ of oven dry |
| 123 | 90∶10 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Roll embrane method | 80 ℃ of oven dry |
| 124 | 90∶10 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Injection moulding | 80 ℃ of oven dry |
| 125 | 90∶10 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Organic curtain coating | 80 ℃ of oven dry |
| 126 | 90∶10 | CaF 2-Y 2O 3Respectively account for 1.0wt% | The gel casting | 80 ℃ of oven dry |
| 127 | 90∶10 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Water-based tape casting | 80 ℃ of oven dry |
| 128 | 90∶10 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Roll embrane method | 80 ℃ of oven dry |
| 129 | 90∶10 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Injection moulding | 80 ℃ of oven dry |
| 130 | 90∶10 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Organic curtain coating | 80 ℃ of oven dry |
| 131 | 90∶10 | CaF 2-Y 2O 3Respectively account for 2.0wt% | The gel casting | 80 ℃ of oven dry |
| 132 | 90∶10 | CaF 2-Y 2O 3Respectively account for 2.0wt% | Water-based tape casting | 80 ℃ of oven dry |
| 133 | 90∶10 | CaF 2-Y 2O 3Respectively account for 2.0wt% | Roll embrane method | 80 ℃ of oven dry |
| 134 | 90∶10 | CaF 2-Y 2O 3Respectively account for 2.0wt% | Injection moulding | 80 ℃ of oven dry |
| 135 | 90∶10 | CaF 2-Y 2O 3Respectively account for 2.0wt% | Organic curtain coating | 80 ℃ of oven dry |
| 136 | 90∶10 | CaF 2-Y 2O 3Respectively account for 0.5wt% | The gel casting | 80 ℃ of oven dry |
| 137 | 90∶10 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Water-based tape casting | 80 ℃ of oven dry |
| 138 | 90∶10 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Roll embrane method | 80 ℃ of oven dry |
| 139 | 90∶10 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Injection moulding | 80 ℃ of oven dry |
| 140 | 90∶10 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Organic curtain coating | 80 ℃ of oven dry |
| 141 | 90∶10 | CaF 2-Y 2O 3Respectively account for 1.0wt% | The gel casting | 80 ℃ of oven dry |
| 142 | 90∶10 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Water-based tape casting | 80 ℃ of oven dry |
| 143 | 90∶10 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Roll embrane method | 70 ℃ of oven dry |
| 144 | 90∶10 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Injection moulding | 70 ℃ of oven dry |
| 145 | 90∶10 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Organic curtain coating | 70 ℃ of oven dry |
| 146 | 90∶10 | CaF 2-Y 2O 3Respectively account for 2.0wt% | The gel casting | 70 ℃ of oven dry |
| 147 | 90∶10 | CaF 2-Y 2O 3Respectively account for 2.0wt% | Water-based tape casting | 70 ℃ of oven dry |
| 148 | 90∶10 | CaF 2-Y 2O 3Respectively account for 2.0wt% | Roll embrane method | 70 ℃ of oven dry |
| 149 | 90∶10 | CaF 2-Y 20 3Respectively account for 2.0wt% | Injection moulding | 70 ℃ of oven dry |
| 150 | 90∶10 | CaF 2-Y 2O 3Respectively account for 2.0wt% | Organic curtain coating | 70 ℃ of oven dry |
| 151 | 80∶20 | CaF 2-Y 2O 3Respectively account for 0.5wt% | The gel casting | 70 ℃ of oven dry |
| 152 | 80∶20 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Water-based tape casting | 70 ℃ of oven dry |
| 153 | 80∶20 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Roll embrane method | 70 ℃ of oven dry |
| 154 | 80∶20 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Injection moulding | 70 ℃ of oven dry |
| 155 | 80∶20 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Organic curtain coating | 70 ℃ of oven dry |
| 156 | 80∶20 | CaF 2-Y 2O 3Respectively account for 1.0wt% | The gel casting | 70 ℃ of oven dry |
| 157 | 80∶20 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Water-based tape casting | 70 ℃ of oven dry |
| 158 | 80∶20 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Roll embrane method | 70 ℃ of oven dry |
| 159 | 80∶20 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Injection moulding | 70 ℃ of oven dry |
| 160 | 80∶20 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Organic curtain coating | 70 ℃ of oven dry |
| 161 | 80∶20 | CaF 2-Y 2O 3Respectively account for 2.0wt% | The gel casting | 70 ℃ of oven dry |
| 162 | 80∶20 | CaF 2-Y 2O 3Respectively account for 2.0wt% | Water-based tape casting | 70 ℃ of oven dry |
| 163 | 80∶20 | CaF 2-Y 2O 3Respectively account for 2.0wt% | Roll embrane method | 70 ℃ of oven dry |
| 164 | 80∶20 | CaF 2-Y 2O 3Respectively account for 2.0wt% | Injection moulding | 70 ℃ of oven dry |
| 165 | 80∶20 | CaF 2-Y 2O 3Respectively account for 2.0wt% | Organic curtain coating | 70 ℃ of oven dry |
| 166 | 75∶25 | CaF 2-Y 2O 3Respectively account for 0.5wt% | The gel casting | 70 ℃ of oven dry |
| 167 | 75∶25 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Water-based tape casting | 60 ℃ of oven dry |
| 168 | 75∶25 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Roll embrane method | 60 ℃ of oven dry |
| 169 | 75∶25 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Injection moulding | 60 ℃ of oven dry |
| 170 | 75∶25 | CaF 2-Y 2O 3Respectively account for 0.5wt% | Organic curtain coating | 60 ℃ of oven dry |
| 171 | 75∶25 | CaF 2-Y 2O 3Respectively account for 1.0wt% | The gel casting | 60 ℃ of oven dry |
| 172 | 75∶25 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Water-based tape casting | 60 ℃ of oven dry |
| 173 | 75∶25 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Roll embrane method | 60 ℃ of oven dry |
| 174 | 75∶25 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Injection moulding | 60 ℃ of oven dry |
| 175 | 75∶25 | CaF 2-Y 2O 3Respectively account for 1.0wt% | Organic curtain coating | 60 ℃ of oven dry |
| 176 | 75∶25 | CaF 2-Y 2O 3Respectively account for 2.0wt% | The gel casting | 60 ℃ of oven dry |
| 177 | 75∶25 | CaF 2-Y 2O 3Respectively account for 2.0wt% | Water-based tape casting | 60 ℃ of oven dry |
| 178 | 75∶25 | CaF 2-Y 2O 3Respectively account for 2.0wt% | Roll embrane method | 60 ℃ of oven dry |
| 179 | 75∶25 | CaF 2-Y 2O 3Respectively account for 2.0wt% | Injection moulding | 60 ℃ of oven dry |
| 180 | 75∶25 | CaF 2-Y 2O 3Respectively account for 2.0wt% | Organic curtain coating | 60 ℃ of oven dry |
Table 1-4 is with the embodiment processing parameter (continued) of calcium oxide as additive
| The embodiment sequence number | Prescription (wt%) | Molding mode | Base sheet drying | |
| Al 2O 3: hydrophilic graphite or carbon black (weight ratio | Auxiliary agent content (wt%) | |||
| 181 | 90∶10 | CaCO 3(in CaO), 0.5% | The gel casting | 80 ℃ of oven dry |
| 182 | 90∶10 | CaCO 3(in CaO), 0.5% | Water-based tape casting | 80 ℃ of oven dry |
| 183 | 90∶10 | CaCO 3(in CaO), 0.5% | Roll embrane method | 80 ℃ of oven dry |
| 184 | 90∶10 | CaCO 3(in CaO), 0.5% | Injection moulding | 80 ℃ of oven dry |
| 185 | 90∶10 | CaCO 3(in CaO), 0.5% | Organic curtain coating | 80 ℃ of oven dry |
| 186 | 90∶10 | CaCO 3(in CaO), 1.0% | The gel casting | 80 ℃ of oven dry |
| 187 | 90∶10 | CaCO 3(in CaO), 1.0% | Water-based tape casting | 80 ℃ of oven dry |
| 188 | 90∶10 | CaCO 3(in CaO), 1.0% | Roll embrane method | 80 ℃ of oven dry |
| 189 | 90∶10 | CaCO 3(in CaO), 1.0% | Injection moulding | 80 ℃ of oven dry |
| 190 | 90∶10 | CaCO 3(in CaO), 1.0% | Organic curtain coating | 80 ℃ of oven dry |
| 191 | 90∶10 | CaCO 3(in CaO), 2.0% | The gel casting | 80 ℃ of oven dry |
| 192 | 90∶10 | CaCO 3(in CaO), 2.0% | Water-based tape casting | 80 ℃ of oven dry |
| 193 | 90∶10 | CaCO 3(in CaO), 2.0% | Roll embrane method | 80 ℃ of oven dry |
| 194 | 90∶10 | CaCO 3(in CaO), 2.0% | Injection moulding | 80 ℃ of oven dry |
| 195 | 90∶10 | CaCO 3(in CaO), 2.0% | Organic curtain coating | 80 ℃ of oven dry |
| 196 | 85∶15 | CaCO 3(in CaO), 0.5% | The gel casting | 80 ℃ of oven dry |
| 197 | 85∶15 | CaCO 3(in CaO), 0.5% | Water-based tape casting | 80 ℃ of oven dry |
| 198 | 85∶15 | CaCO 3(in CaO), 0.5% | Roll embrane method | 80 ℃ of oven dry |
| 199 | 85∶15 | CaCO 3(in CaO), 0.5% | Injection moulding | 80 ℃ of oven dry |
| 200 | 85∶15 | CaCO 3(in CaO), 0.5% | Organic curtain coating | 80 ℃ of oven dry |
| 201 | 85∶15 | CaCO 3(in CaO), 1.0% | The gel casting | 80 ℃ of oven dry |
| 202 | 85∶15 | CaCO 3(in CaO), 1.0% | Water-based tape casting | 80 ℃ of oven dry |
| 203 | 85∶15 | CaCO 3(in CaO), 1.0% | Roll embrane method | 80 ℃ of oven dry |
| 204 | 85∶15 | CaCO 3(in CaO), 1.0% | Injection moulding | 80 ℃ of oven dry |
| 205 | 85∶15 | CaCO 3(in CaO), 1.0% | Organic curtain coating | 80 ℃ of oven dry |
| 206 | 85∶15 | CaCO 3(in CaO), 2.0% | The gel casting | 80 ℃ of oven dry |
| 207 | 85∶15 | CaCO 3(in CaO), 2.0% | Water-based tape casting | 80 ℃ of oven dry |
| 208 | 85∶15 | CaCO 3(in CaO), 2.0% | Roll embrane method | 80 ℃ of oven dry |
| 209 | 85∶15 | CaCO 3(in CaO), 2.0% | Injection moulding | 80 ℃ of oven dry |
| 210 | 85∶15 | CaCO 3(in CaO), 2.0% | Organic curtain coating | 80 ℃ of oven dry |
| 211 | 80∶20 | CaCO 3(in CaO), 0.5% | The gel casting | 80 ℃ of oven dry |
| 212 | 80∶20 | CaCO 3(in CaO), 0.5% | Water-based tape casting | 80 ℃ of oven dry |
| 213 | 80∶20 | CaCO 3(in CaO), 0.5% | Roll embrane method | 80 ℃ of oven dry |
| 214 | 80∶20 | CaCO 3(in CaO), 0.5% | Injection moulding | 80 ℃ of oven dry |
| 215 | 80∶20 | CaCO 3(in CaO), 0.5% | Organic curtain coating | 80 ℃ of oven dry |
| 216 | 80∶20 | CaCO 3(in CaO), 1.0% | The gel casting | 80 ℃ of oven dry |
| 217 | 80∶20 | CaCO 3(in CaO), 1.0% | Water-based tape casting | 80 ℃ of oven dry |
| 218 | 80∶20 | CaCO 3(in CaO), 1.0% | Roll embrane method | 80 ℃ of oven dry |
| 219 | 80∶20 | CaCO 3(in CaO), 1.0% | Injection moulding | 80 ℃ of oven dry |
| 220 | 80∶20 | CaCO 3(in CaO), 1.0% | Organic curtain coating | 80 ℃ of oven dry |
| 221 | 80∶20 | CaCO 3(in CaO), 2.0% | The gel casting | 80 ℃ of oven dry |
| 222 | 80∶20 | CaCO 3(in CaO), 2.0% | Water-based tape casting | 80 ℃ of oven dry |
| 223 | 80∶20 | CaCO 3(in CaO), 2.0% | Roll embrane method | 80 ℃ of oven dry |
| 224 | 80∶20 | CaCO 3(in CaO), 2.0% | Injection moulding | 80 ℃ of oven dry |
| 225 | 80∶20 | CaCO 3(in CaO), 2.0% | Organic curtain coating | 80 ℃ of oven dry |
| 226 | 75∶25 | CaCO 3(in CaO), 0.5% | The gel casting | 80 ℃ of oven dry |
| 227 | 75∶25 | CaCO 3(in CaO), 0.5% | Water-based tape casting | 80 ℃ of oven dry |
| 228 | 75∶25 | CaCO 3(in CaO), 0.5% | Roll embrane method | 80 ℃ of oven dry |
| 229 | 75∶25 | CaCO 3(in CaO), 0.5% | Injection moulding | 80 ℃ of oven dry |
| 230 | 75∶25 | CaCO 3(in CaO), 0.5% | Organic curtain coating | 80 ℃ of oven dry |
| 231 | 75∶25 | CaCO 3(in CaO), 1.0% | The gel casting | 80 ℃ of oven dry |
| 232 | 75∶25 | CaCO 3(in CaO), 1.0% | Water-based tape casting | 80 ℃ of oven dry |
| 233 | 75∶25 | CaCO 3(in CaO), 1.0% | Roll embrane method | 80 ℃ of oven dry |
| 234 | 75∶25 | CaCO 3(in CaO), 1.0% | Injection moulding | 80 ℃ of oven dry |
| 235 | 75∶25 | CaCO 3(in CaO), 1.0% | Organic curtain coating | 80 ℃ of oven dry |
| 236 | 75∶25 | CaCO 3(in CaO), 2.0% | The gel casting | 80 ℃ of oven dry |
| 237 | 75∶25 | CaCO 3(in CaO), 2.0% | Water-based tape casting | 80 ℃ of oven dry |
| 238 | 75∶25 | CaCO 3(in CaO), 2.0% | Roll embrane method | 80 ℃ of oven dry |
| 239 | 75∶25 | CaCO 3(in CaO), 2.0% | Injection moulding | 80 ℃ of oven dry |
| 240 | 75∶25 | CaCO 3(in CaO), 2.0% | Organic curtain coating | 80 ℃ of oven dry |
Table 1-5 is with the embodiment processing parameter (continued) of Calcium Fluoride (Fluorspan)-yttrium fluoride as additive
| The embodiment sequence number | Prescription (wt%) | Molding mode | Base sheet drying | |
| Al 2O 3: hydrophilic graphite or carbon black (weight ratio | Auxiliary agent content (wt%) | |||
| 241 | 90∶10 | CaF 2-YF 3Respectively account for 0.5wt% | The gel casting | 80 ℃ of oven dry |
| 242 | 90∶10 | CaF 2-YF 3Respectively account for 0.5wt% | Water-based tape casting | 80 ℃ of oven dry |
| 243 | 90∶10 | CaF 2-YF 3Respectively account for 0.5wt% | Roll embrane method | 80 ℃ of oven dry |
| 244 | 90∶10 | CaF 2-YF 3Respectively account for 0.5wt% | Injection moulding | 80 ℃ of oven dry |
| 245 | 90∶10 | CaF 2-YF 3Respectively account for 0.5wt% | Organic curtain coating | 80 ℃ of oven dry |
| 246 | 90∶10 | CaF 2-YF 3Respectively account for 1.0wt% | The gel casting | 80 ℃ of oven dry |
| 247 | 90∶10 | CaF 2-YF 3Respectively account for 1.0wt% | Water-based tape casting | 80 ℃ of oven dry |
| 248 | 90∶10 | CaF 2-YF 3Respectively account for 1.0wt% | Roll embrane method | 80 ℃ of oven dry |
| 249 | 90∶10 | CaF 2-YF 3Respectively account for 1.0wt% | Injection moulding | 80 ℃ of oven dry |
| 250 | 90∶10 | CaF 2-YF 3Respectively account for 1.0wt% | Organic curtain coating | 80 ℃ of oven dry |
| 251 | 90∶10 | CaF 2-YF 3Respectively account for 2.0wt% | The gel casting | 80 ℃ of oven dry |
| 252 | 90∶10 | CaF 2-YF 3Respectively account for 2.0wt% | Water-based tape casting | 80 ℃ of oven dry |
| 253 | 90∶10 | CaF 2-YF 3Respectively account for 2.0wt% | Roll embrane method | 80 ℃ of oven dry |
| 254 | 90∶10 | CaF 2-YF 3Respectively account for 2.0wt% | Injection moulding | 80 ℃ of oven dry |
| 255 | 90∶10 | CaF 2-YF 3Respectively account for 2.0wt% | Organic curtain coating | 80 ℃ of oven dry |
| 256 | 85∶15 | CaF 2-YF 3Respectively account for 0.5wt% | The gel casting | 80 ℃ of oven dry |
| 257 | 85∶15 | CaF 2-YF 3Respectively account for 0.5wt% | Water-based tape casting | 80 ℃ of oven dry |
| 258 | 85∶15 | CaF 2-YF 3Respectively account for 0.5wt% | Roll embrane method | 70 ℃ of oven dry |
| 259 | 85∶15 | CaF 2-YF 3Respectively account for 0.5wt% | Injection moulding | 70 ℃ of oven dry |
| 260 | 85∶15 | CaF 2-YF 3Respectively account for 0.5wt% | Organic curtain coating | 70 ℃ of oven dry |
| 261 | 85∶15 | CaF 2-YF 3Respectively account for 1.0wt% | The gel casting | 70 ℃ of oven dry |
| 262 | 85∶15 | CaF 2-YF 3Respectively account for 1.0wt% | Water-based tape casting | 70 ℃ of oven dry |
| 263 | 85∶15 | CaF 2-YF 3Respectively account for 1.0wt% | Roll embrane method | 70 ℃ of oven dry |
| 264 | 85∶15 | CaF 2-YF 3Respectively account for 1.0wt% | Injection moulding | 70 ℃ of oven dry |
| 265 | 85∶15 | CaF 2-YF 3Respectively account for 1.0wt% | Organic curtain coating | 70 ℃ of oven dry |
| 266 | 85∶15 | CaF 2-YF 3Respectively account for 2.0wt% | The gel casting | 70 ℃ of oven dry |
| 267 | 85∶15 | CaF 2-YF 3Respectively account for 2.0wt% | Water-based tape casting | 70 ℃ of oven dry |
| 268 | 85∶15 | CaF 2-YF 3Respectively account for 2.0wt% | Roll embrane method | 70 ℃ of oven dry |
| 269 | 85∶15 | CaF 2-YF 3Respectively account for 2.0wt% | Injection moulding | 70 ℃ of oven dry |
| 270 | 85∶15 | CaF 2-YF 3Respectively account for 2.0wt% | Organic curtain coating | 70 ℃ of oven dry |
| 271 | 80∶20 | CaF 2-YF 3Respectively account for 0.5wt% | The gel casting | 70 ℃ of oven dry |
| 272 | 80∶20 | CaF 2-YF 3Respectively account for 0.5wt% | Water-based tape casting | 70 ℃ of oven dry |
| 273 | 80∶20 | CaF 2-YF 3Respectively account for 0.5wt% | Roll embrane method | 70 ℃ of oven dry |
| 274 | 80∶20 | CaF 2-YF 3Respectively account for 0.5wt% | Injection moulding | 70 ℃ of oven dry |
| 275 | 80∶20 | CaF 2-YF 3Respectively account for 0.5wt% | Organic curtain coating | 70 ℃ of oven dry |
| 276 | 80∶20 | CaF 2-YF 3Respectively account for 1.0wt% | The gel casting | 70 ℃ of oven dry |
| 277 | 80∶20 | CaF 2-YF 3Respectively account for 1.0wt% | Water-based tape casting | 70 ℃ of oven dry |
| 278 | 80∶20 | CaF 2-YF 3Respectively account for 1.0wt% | Roll embrane method | 70 ℃ of oven dry |
| 279 | 80∶20 | CaF 2-YF 3Respectively account for 1.0wt% | Injection moulding | 70 ℃ of oven dry |
| 280 | 80∶20 | CaF 2-YF 3Respectively account for 1.0wt% | Organic curtain coating | 70 ℃ of oven dry |
| 281 | 80∶20 | CaF 2-YF 3Respectively account for 2.0wt% | The gel casting | 70 ℃ of oven dry |
| 282 | 80∶20 | CaF 2-YF 3Respectively account for 2.0wt% | Water-based tape casting | 70 ℃ of oven dry |
| 283 | 80∶20 | CaF 2-YF 3Respectively account for 2.0wt% | Roll embrane method | 80 ℃ of oven dry |
| 284 | 80∶20 | CaF 2-YF 3Respectively account for 2.0wt% | Injection moulding | 80 ℃ of oven dry |
| 285 | 80∶20 | CaF 2-YF 3Respectively account for 2.0wt% | Organic curtain coating | 80 ℃ of oven dry |
| 286 | 75∶25 | CaF 2-YF 3Respectively account for 0.5wt% | The gel casting | 80 ℃ of oven dry |
| 287 | 75∶25 | CaF 2-YF 3Respectively account for 0.5wt% | Water-based tape casting | 80 ℃ of oven dry |
| 288 | 75∶25 | CaF 2-YF 3Respectively account for 0.5wt% | Roll embrane method | 80 ℃ of oven dry |
| 289 | 75∶25 | CaF 2-YF 3Respectively account for 0.5wt% | Injection moulding | 80 ℃ of oven dry |
| 290 | 75∶25 | CaF 2-YF 3Respectively account for 0.5wt% | Organic curtain coating | 80 ℃ of oven dry |
| 291 | 75∶25 | CaF 2-YF 3Respectively account for 1.0wt% | The gel casting | 80 ℃ of oven dry |
| 292 | 75∶25 | CaF 2-YF 3Respectively account for 1.0wt% | Water-based tape casting | 80 ℃ of oven dry |
| 293 | 75∶25 | CaF 2-YF 3Respectively account for 1.0wt% | Roll embrane method | 80 ℃ of oven dry |
| 294 | 75∶25 | CaF 2-YF 3Respectively account for 1.0wt% | Injection moulding | 80 ℃ of oven dry |
| 295 | 75∶25 | CaF 2-YF 3Respectively account for 1.0wt% | Organic curtain coating | 80 ℃ of oven dry |
| 296 | 75∶25 | CaF 2-YF 3Respectively account for 2.0wt% | The gel casting | 80 ℃ of oven dry |
| 297 | 75∶25 | CaF 2-YF 3Respectively account for 2.0wt% | Water-based tape casting | 80 ℃ of oven dry |
| 298 | 75∶25 | CaF 2-YF 3Respectively account for 2.0wt% | Roll embrane method | 80 ℃ of oven dry |
| 299 | 75∶25 | CaF 2-YF 3Respectively account for 2.0wt% | Injection moulding | 80 ℃ of oven dry |
| 300 | 75∶25 | CaF 2-YF 3Respectively account for 2.0wt% | Organic curtain coating | 80 ℃ of oven dry |
Table 2-1 is with the embodiment processing parameter (continuous table 1-1) of Calcium Fluoride (Fluorspan) as additive
| The embodiment sequence number | Carbothermal reduction-nitridation technology | The carbon residue burn off | Rubbing down | Cover flat |
| 1 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 2 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 3 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 4 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 5 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 6 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 7 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 8 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 9 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 10 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 11 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 12 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 13 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 14 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 15 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 16 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 17 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 18 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 19 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 20 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 21 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 22 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 23 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 24 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 25 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 26 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 27 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 28 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 29 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 30 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 31 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 32 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 33 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 34 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 35 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 36 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 37 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 38 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 39 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 40 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 41 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 42 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 43 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 44 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 45 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 46 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 47 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 48 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 49 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 50 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 51 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 52 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 53 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 54 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 55 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 56 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 57 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 58 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 59 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 60 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
Table 2-2 is with the embodiment processing parameter (continuous table 1-2) of yttrium oxide as additive
| The embodiment sequence number | Carbothermal reduction-nitridation technology | The carbon residue burn off | Rubbing down | Cover flat |
| 61 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 62 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 63 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 64 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 65 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 66 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 67 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 68 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 69 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 70 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 71 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 72 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 73 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 74 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 75 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 76 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 77 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 78 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 79 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 80 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 81 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 82 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 83 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 84 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 85 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 86 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 87 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 88 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 89 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 90 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 91 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 92 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 93 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 94 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 95 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 96 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 97 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 98 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 99 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 100 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 101 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 102 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 103 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 104 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 105 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 106 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 107 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 108 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 109 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 110 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 111 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 112 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 113 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 114 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 115 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 116 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 117 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 118 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 119 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 120 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
Table 2-3 is with the embodiment processing parameter (continuous table 1-3) of Calcium Fluoride (Fluorspan)-yttrium oxide as additive
| The embodiment sequence number | Carbothermal reduction-nitridation technology | The carbon residue burn off | Rubbing down | Cover flat |
| 121 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 122 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 123 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 124 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 125 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 126 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 127 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 128 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 129 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 130 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 131 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 132 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 133 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 134 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 135 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 136 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 137 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 138 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 139 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 140 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 141 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 142 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 143 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 144 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 145 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 146 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 147 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 148 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 149 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 150 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 151 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 152 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 153 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 154 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 155 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 156 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 157 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 158 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 159 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 160 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 161 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 162 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 163 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 164 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 165 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 166 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 167 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 168 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 169 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 170 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 171 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 172 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 173 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 174 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 175 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 176 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 177 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 178 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 179 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 180 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
Table 2-4 is with the embodiment processing parameter (continuous table 1-4) of calcium oxide as additive
| The embodiment sequence number | Carbothermal reduction-nitridation technology | The carbon residue burn off | Rubbing down | Cover flat |
| 181 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 182 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 183 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 184 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 185 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 186 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 187 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 188 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 189 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 190 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 191 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 192 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 193 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 194 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 195 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 196 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 197 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 198 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 199 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 200 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 201 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 202 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 203 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 204 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 205 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 206 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 207 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 208 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 209 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 210 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 211 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 212 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 213 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 214 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 215 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 216 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 217 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 218 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 219 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 220 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 221 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 222 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 223 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 224 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 225 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 226 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 227 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 228 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 229 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 230 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 231 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 232 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 233 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 234 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 235 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 236 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 237 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 238 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 239 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 240 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
Table 2-5 is with the embodiment processing parameter (continuous table 1-5) of Calcium Fluoride (Fluorspan)-yttrium fluoride as additive
| The embodiment sequence number | Carbothermal reduction-nitridation technology | The carbon residue burn off | Rubbing down | Cover flat |
| 241 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 242 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 243 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 244 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 245 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 246 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 247 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 248 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 249 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 250 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 251 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 252 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 253 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 254 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 255 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 256 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 257 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 258 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 259 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 260 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 261 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 262 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 263 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 264 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 265 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 266 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 267 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 268 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 269 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 270 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 271 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 272 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 273 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 274 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 275 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 276 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 277 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 278 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 279 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 280 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 281 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 282 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 283 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 284 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 285 | 1750℃，3h | 700℃，3h | Use SiC sand rubbing down in the water | 1600℃，2h |
| 286 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 287 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 288 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 289 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 290 | 1700℃，4h | 700℃，3h | Use SiC sand rubbing down in the water | 1550℃，2h |
| 291 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 292 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 293 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 294 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 295 | 1650℃，5h | 700℃，3h | Use SiC sand rubbing down in the water | 1520℃，2h |
| 296 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 297 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 298 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 299 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
| 300 | 1600℃，6h | 700℃，3h | Use SiC sand rubbing down in the water | 1500℃，2h |
Claims (1)
1, a kind of method for preparing aluminium nitride ceramic substrate is characterized in that, utilizes aluminum oxide and wetting ability graphite or carbon black to prepare aluminium nitride ceramic substrate for main raw material, and its processing step is as follows:
1.1, batching, according to the composition requirement of prepared ceramic green sheet, accurate weighing aluminum oxide powder powder stock; Take by weighing reaction promoter, it is CaF
2, Y
2O
3, YF
6, CaO, CaCO
3, BN one of them or the wherein combination of several materials, promoter addition is 0.5～5wt% of alumina powder weight; Take by weighing wetting ability graphite or carbon black powder, its add-on is the 10wt%～25wt% of alumina powder,
1.2, the moulding of base sheet, one of following method is adopted in the moulding of base sheet: gel is cast type, injection moulding, rolling formation, organic flow casting molding, aqueous tape casting forming,
1.3, base sheet drying, after slurry gelization was finished, disengageding mould was positioned over base substrate on the gas-pervious mesh screen or on the smooth plasterboard it is dehydrated, drying mode adopts seasoning, blowing drying or heat drying,
1.4, the lamination that sands, onesize ceramic green sheet is stacked together, 1～15 every pile, spill one deck corundum sand between sheet and the sheet equably, snarl with adhesive tape then,
1.5, carbothermal reduction-nitridation reaction, the ceramic green sheet that has spread sand is placed on N
2Carry out carbothermic reduction reaction in the atmosphere furnace, wherein, N
2Flow is 1～5L/min, and temperature rise rate is controlled at 5～20 ℃, at first is raised to 500～700 ℃ of insulation 0.5～5h, is warmed up to 1600～1800 ℃ of insulation 2～8h then, come out of the stove when being cooled at last not be higher than 200 ℃,
1.6, the carbon residue burn off, the porcelain body of coming out of the stove in the nitrogen furnace is placed on carries out the carbon residue burn off in the air furnace and handle, technological temperature is 600～800 ℃, soaking time 2～10h,
1.7, rubbing down removes parting sand, will finish ceramic plate behind the carbon residue burn off and in water, carry out rubbing down and handle, with the isolation sand on removing ceramics surface,
1.8, cover flat the processing, ceramics covers flat the processing under nitrogen atmosphere the most at last, guarantees the planeness of substrate, wherein, covers to put down being lower than under 200～300 ℃ of the sintering temperatures and carries out, covering at ordinary times, soaking time is 2～4h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01142028 CN1207247C (en) | 2001-09-07 | 2001-09-07 | Prepn process of aluminium nitride ceramic substrate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01142028 CN1207247C (en) | 2001-09-07 | 2001-09-07 | Prepn process of aluminium nitride ceramic substrate |
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|---|---|
| CN1403409A CN1403409A (en) | 2003-03-19 |
| CN1207247C true CN1207247C (en) | 2005-06-22 |
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|---|---|---|---|
| CN 01142028 Expired - Fee Related CN1207247C (en) | 2001-09-07 | 2001-09-07 | Prepn process of aluminium nitride ceramic substrate |
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Families Citing this family (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304334C (en) * | 2004-05-24 | 2007-03-14 | Tdk株式会社 | Imbarking plate, ceramic base-plate manufacturing method and ceramic base-plate |
| CN100398432C (en) * | 2004-12-22 | 2008-07-02 | 台盐实业股份有限公司 | Method for synthesizing aluminium nitride |
| CN102030538B (en) * | 2009-09-30 | 2013-04-10 | 比亚迪股份有限公司 | Production method of aluminum nitride ceramic and aluminum nitride ceramic prepared by same |
| WO2012055206A1 (en) * | 2010-10-26 | 2012-05-03 | Yu Jianping | Alumina/graphite composite ceramic material and led light source utilizing the material as substrate |
| CN102732853B (en) * | 2011-04-08 | 2014-12-17 | 北京北方微电子基地设备工艺研究中心有限责任公司 | Chamber device and substrate-processing device therewith |
| CN102716700B (en) | 2012-06-18 | 2014-07-16 | 南京工业大学 | Preparation method for high-strength heat-resisting massive C-AlN compound aerogel |
| CN104649677A (en) * | 2013-11-18 | 2015-05-27 | 北京大学 | A method of preparing an aluminium nitride ceramic substrate by gel casting |
| CN104227827B (en) * | 2014-09-11 | 2017-06-06 | 瑞声精密制造科技(常州)有限公司 | The forming method of ceramic product |
| CN106316466A (en) * | 2015-06-15 | 2017-01-11 | 长沙市望城区启天陶瓷有限公司 | Making method of multilayer ceramic |
| CN106744739B (en) * | 2016-12-21 | 2019-02-15 | 潮州三环（集团）股份有限公司 | The preparation method of aluminium nitride powder |
| CN107263671B (en) * | 2017-06-27 | 2019-06-18 | 江苏德纳化学股份有限公司 | A kind of preparation method of the composite modified aluminium nitride chip of resistance to shrinkage type of twin crystal palpus |
| CN107986794A (en) * | 2017-11-29 | 2018-05-04 | 上海大学 | The preparation method of large scale aluminum nitride ceramic substrate |
| CN110143818B (en) * | 2018-02-12 | 2021-09-03 | 比亚迪股份有限公司 | Preparation method of ceramic shell and ceramic shell |
| CN111517803B (en) * | 2020-04-25 | 2020-12-08 | 湖南省美程陶瓷科技有限公司 | Ceramic support for microwave magnetron and preparation method thereof |
| CN116410001A (en) * | 2021-12-31 | 2023-07-11 | 江苏博睿光电股份有限公司 | Substrate, preparation method and application |
| CN115304383A (en) * | 2022-08-19 | 2022-11-08 | 广东省先进陶瓷材料科技有限公司 | Aluminum nitride substrate and preparation method and application thereof |
| CN116425552B (en) * | 2023-04-24 | 2024-04-26 | 广东省先进陶瓷材料科技有限公司 | Aluminum nitride substrate and preparation method and application thereof |
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