CN117401982A - Preparation method of silicon oxynitride ceramic lift tube - Google Patents
Preparation method of silicon oxynitride ceramic lift tube Download PDFInfo
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- CN117401982A CN117401982A CN202311399288.XA CN202311399288A CN117401982A CN 117401982 A CN117401982 A CN 117401982A CN 202311399288 A CN202311399288 A CN 202311399288A CN 117401982 A CN117401982 A CN 117401982A
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- silicon oxynitride
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- lift tube
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- 239000000919 ceramic Substances 0.000 title claims abstract description 91
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 73
- 239000010703 silicon Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 47
- 238000005245 sintering Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000000498 ball milling Methods 0.000 claims abstract description 18
- 239000002002 slurry Substances 0.000 claims abstract description 15
- 238000004806 packaging method and process Methods 0.000 claims abstract description 9
- 238000001694 spray drying Methods 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000004615 ingredient Substances 0.000 claims abstract description 5
- 238000000465 moulding Methods 0.000 claims abstract description 5
- 239000000654 additive Substances 0.000 claims abstract description 4
- 230000000996 additive effect Effects 0.000 claims abstract description 4
- 238000001514 detection method Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 27
- YQNQTEBHHUSESQ-UHFFFAOYSA-N lithium aluminate Chemical compound [Li+].[O-][Al]=O YQNQTEBHHUSESQ-UHFFFAOYSA-N 0.000 claims description 25
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 24
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 22
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 22
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 18
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 16
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 12
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000011230 binding agent Substances 0.000 claims description 11
- 239000002270 dispersing agent Substances 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 9
- 238000000462 isostatic pressing Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000010298 pulverizing process Methods 0.000 claims description 9
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 8
- 239000011787 zinc oxide Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 6
- 238000003754 machining Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 5
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 3
- 239000001095 magnesium carbonate Substances 0.000 claims description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 238000009740 moulding (composite fabrication) Methods 0.000 abstract 1
- 229910000838 Al alloy Inorganic materials 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 9
- 239000007788 liquid Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 230000035939 shock Effects 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 238000005266 casting Methods 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 229910001018 Cast iron Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229910000505 Al2TiO5 Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000001089 mineralizing effect Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- AABBHSMFGKYLKE-SNAWJCMRSA-N propan-2-yl (e)-but-2-enoate Chemical compound C\C=C\C(=O)OC(C)C AABBHSMFGKYLKE-SNAWJCMRSA-N 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004512 die casting Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/597—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon oxynitride, e.g. SIALONS
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Abstract
The invention provides a preparation method of a silicon oxynitride ceramic lift tube, which comprises the following steps: selecting ingredients, adding the ingredients into a stirring mill, and ball-milling for 22-26 hours to prepare uniform ceramic slurry; ageing and defoaming the prepared ceramic slurry for 22 to 26 hours, and spray-drying the ceramic slurry by a spray-drying tower to prepare ceramic powder conforming to the granularity grading; after the prepared ceramic powder is aged for more than 48 hours, homogenizing for 30 minutes by using a homogenizer, and adding a molding additive; sintering the ceramic powder into a ceramic silicon oxynitride lift tube; adopting a grinder to process the burned silicon oxynitride lift tube to a designed size, and packaging and warehousing after the detection is qualified; according to the preparation method of the silicon oxynitride ceramic lift tube, provided by the invention, the formula is optimized, and the sintering, ball milling and forming processes are optimized, so that the flexural strength of the lift tube reaches about 400-500 megapascals, and the requirements of the domestic ceramic lift tube can be completely met.
Description
Technical Field
The invention belongs to the technical field of preparation methods of silicon oxynitride ceramic lift tubes, and particularly relates to a preparation method of a silicon oxynitride ceramic lift tube.
Background
The liquid lifting pipe used in the aluminum casting industry is one of key components on a low-pressure casting machine, and the performance and stability of the liquid lifting pipe directly influence the quality and production efficiency of a cast product.
The working principle of the lift tube is generally as follows: the lower end is inserted into the aluminum alloy melt of the heat preservation furnace, the upper end is connected with a casting mold cavity, and the aluminum alloy melt enters the mold cavity from bottom to top under the action of pressure to complete casting; the liquid lifting pipe has good thermal shock resistance, corrosion resistance to aluminum alloy melt, no wetting with the aluminum alloy melt, good air tightness and thermal shock fatigue resistance according to the working condition requirements.
In the prior art, the main lift tube is a cast iron lift tube, an aluminum titanate lift tube and a silicon nitride ceramic lift tube; however, the cast iron lift tube is not resistant to corrosion of aluminum alloy melt in use, cast iron impurities are easy to add to an aluminum alloy casting, the service life is short, and the production efficiency is affected; the synthesis and sintering temperature of the aluminum titanate ceramic are not easy to control, the strength is not high, and the service life is two months; the silicon nitride ceramic lift tube is corrosion-resistant, has relatively general thermal shock resistance, and has slight reaction with aluminum alloy melt with high magnesium and zinc content, and the service life is about one year.
Based on the technical problems existing in the lift tube, no relevant solution exists; there is therefore an urgent need to seek an effective solution to the above problems.
Disclosure of Invention
The invention aims to solve the problems of insufficient thermal shock resistance, short service life and poor high-temperature corrosion resistance of an aluminum alloy melt of the existing lift tube.
The invention provides a preparation method of a silicon oxynitride ceramic lift tube, which comprises the following steps:
s1: the selecting ingredients comprise:
80-90 parts of silicon oxynitride powder;
1-3 parts of calcined alumina;
2-6 parts of lithium aluminate;
1-5 parts of sintering aid;
1 part of dispersing agent;
3 parts of binder PVB;
100-150 parts of ethanol;
s2: proportioning and ball milling: adding the silicon oxynitride powder, the calcined alumina, the lithium aluminate, the sintering aid, the dispersing agent, the binder PVB and the ethanol selected in the step S1 into a stirring mill, and ball-milling for 22-26 hours to prepare uniform ceramic slurry;
s3: spray pulverizing: ageing and defoaming the prepared ceramic slurry for 22 to 26 hours, and spray-drying the ceramic slurry by a spray-drying tower to prepare ceramic powder conforming to the granularity grading; the moisture of the ceramic powder is controlled below 1%;
s4: homogenizing ceramic powder: after the prepared ceramic powder is aged for more than 48 hours, homogenizing for 30 minutes by using a homogenizer, adding a molding additive, and sub-packaging for later use;
s5: sintering of ceramics: sintering the ceramic powder in the step S4 into a ceramic silicon oxynitride lift tube; slowly heating up at the speed of 50 ℃ per hour, slowing down the heating up speed to 40 to 48 ℃ per hour at 300 to 400 ℃ and preserving heat for 6 hours at 300 to 400 ℃, then continuously heating up to 1650 ℃, preserving heat for 3 hours, and naturally cooling to normal temperature;
s6: processing and detecting: and (3) processing the burned silicon oxynitride lift tube to a designed size by adopting a grinding machine, and packaging and warehousing after the detection is qualified.
Further, S4 further includes isostatic pressing forming and lathe processing:
s41: placing the homogenized ceramic powder into an isostatic pressing die, sealing and fastening by using rubber bands, and placing into an isostatic pressing machine;
s42: pressurizing to 300MPa, maintaining the pressure for 120 seconds, slowly releasing pressure, taking out the formed green body, putting the green body into a drying room at 50 ℃ for drying, putting the green body into a machining equipment machine tool for machining according to the design size after one week of standing.
Further, the pretreatment of lithium aluminate in S1 includes: and (3) mixing the lithium carbonate and the aluminum hydroxide according to a preset molar ratio, respectively adding the mixture into a ball mill, ball milling the mixture with ethanol as a solvent, ball milling the mixture for 24 hours, discharging the mixture, drying the mixture, and calcining the mixture at 1250 ℃ for 6 hours to obtain the lithium aluminate block.
Further, in the pretreatment process of lithium aluminate: the preset molar ratio of the lithium carbonate to the aluminum hydroxide is 1:1, 1:2 and 1:3; crushing the burned lithium aluminate blocks into particles with the diameter of less than 1 mm, mixing the particles with ethanol, ball-grinding the particles into slurry with the diameter of less than 1 micron, drying, pulverizing, and packaging and marking; the preset molar ratio of lithium carbonate to aluminum hydroxide is 1:1 and is recorded as an A1 raw material, the preset molar ratio of lithium carbonate to aluminum hydroxide is 1:2 and is recorded as an A2 raw material, and the preset molar ratio of lithium carbonate to aluminum hydroxide is 1:2 and is recorded as an A3 raw material.
Further, the proportion of the lithium aluminate in S1 is selected to be 3-6 parts or 2-5 parts.
Further, the sintering aid comprises iron oxide, yttrium oxide, barium carbonate, and zinc oxide.
Further, the silicon oxynitride powder is self-propagating synthesized silicon oxynitride; the granularity D50 of the silicon oxynitride powder is less than 3 microns, the silicon oxynitride content is not less than 98%, and the silicon nitride content is not more than 2%.
Further, the calcined alumina is microcrystalline alumina calcined using a mineralizer, and the calcination temperature is lower than 1300 ℃; the alpha phase content of the microcrystalline alumina is not less than 98%; the primary crystal size of the microcrystalline alumina is lower than 100 nanometers; after the calcination and the pulverization, the grain size D50 of the microcrystalline alumina is controlled to be 0.3-0.6 microns.
Further, the aluminum hydroxide is selected from superfine powder with more than 1 ten thousand meshes, the content of aluminum oxide is more than 64 percent, and the content of alkali is less than 0.2 percent.
Further, the lithium carbonate is selected from chemically pure lithium carbonate; s1, mineralizing agent, wherein the mineralizing agent is selected from chemically pure kaolin, basic magnesium carbonate, ferric oxide, zinc oxide, barium carbonate, yttrium oxide, cerium oxide and lanthanum oxide; the granularity of mineralizer is controlled below 1 micron.
Further, the dispersant is ammonium polyacrylate 9300.
Further, the binder is PVB
According to the preparation method of the silicon oxynitride ceramic lift tube, the low liquid phase point materials are adopted for compatibility, the sintering temperature is 1650 ℃, and the problem of high-temperature decomposition of silicon oxynitride is effectively solved by optimizing a ball milling process, a forming process and a sintering process, so that the breaking strength of the lift tube reaches about 400-500 megapascals; the self-propagating powder is adopted, the self-propagating powder is stable in production and quality, the large-scale mass production of the silicon oxynitride ceramic lift tube is possible, and the requirements of the domestic ceramic lift tube can be completely met.
Drawings
The invention will be described in further detail with reference to the drawings and the detailed description.
The invention will be further described with reference to the accompanying drawings in which:
FIG. 1 is a flow chart of a method for preparing a silicon oxynitride ceramic lift tube according to the present invention.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
It will be understood that when an element is referred to as being "mounted" or "disposed" on another element, it can be directly on the other element or be indirectly on the other element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or be indirectly connected to the other element.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present invention, the meaning of "a plurality" is two or more, unless explicitly defined otherwise. The meaning of "a number" is one or more than one unless specifically defined otherwise.
In the description of the present invention, it should be understood that the directions or positional relationships indicated by the terms "upper", "lower", "front", "rear", "left", "right", etc., are based on the directions or positional relationships shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
As shown in fig. 1, the embodiment of the invention provides a preparation method of a silicon oxynitride ceramic lift tube, in particular to a preparation method of a silicon oxynitride ceramic lift tube by using silicon oxynitride powder by a self-propagating method; in the scheme, the silicon oxynitride ceramic has excellent thermal shock resistance, high-temperature non-wettability of aluminum alloy melt, excellent oxidation resistance and excellent high-temperature aluminum alloy melt corrosion resistance, and is an excellent material for preparing a liquid lifting tube for the aluminum die casting industry; specifically, the preparation method comprises the following steps:
s1: the selecting ingredients comprise:
80-90 parts of silicon oxynitride powder;
1-3 parts of calcined alumina;
2-6 parts of lithium aluminate;
1-5 parts of sintering aid;
1 part of dispersing agent;
3 parts of binder PVB;
100-150 parts of ethanol;
s2: proportioning and ball milling: adding the silicon oxynitride powder, the calcined alumina, the lithium aluminate, the sintering aid, the dispersing agent, the binder PVB and the ethanol selected in the step S1 into a stirring mill, and ball-milling for 22-26 hours to prepare uniform ceramic slurry;
s3: spray pulverizing: ageing and defoaming the prepared ceramic slurry for 22 to 26 hours, and spray-drying the ceramic slurry by a spray-drying tower to prepare ceramic powder conforming to the granularity grading; specifically, the moisture of the ceramic powder is controlled below 1%;
s4: homogenizing ceramic powder: after the prepared ceramic powder is aged for more than 48 hours, homogenizing for 30 minutes by using a V-shaped homogenizer, and adding a molding additive to facilitate molding and processing of green bodies and subpackaging for later use;
s5: sintering of ceramics: because the silicon oxynitride lift tube is basically a ceramic large piece, and the weight of each piece is about 20 kg, the sintering of the silicon oxynitride ceramic is the key of the whole process; because in this step: sintering the ceramic powder homogenized in the step S4 into a ceramic silicon oxynitride lift tube; specifically, the sintering is slowly heated up at the speed of 50 ℃ per hour, and the heating up speed is slowed down to 40 to 48 ℃ per hour at 300 to 400 ℃ so as to ensure the glue discharge of the silicon oxynitride ceramic lift tube; keeping the temperature at 500-700 ℃ for 6 hours, then continuously heating to 1650 ℃, keeping the temperature for 3 hours, and naturally cooling to normal temperature; the material formula of the preparation method of the silicon oxynitride ceramic lift tube also enables the sintering temperature to be lower than the decomposition temperature of silicon oxynitride by 1700 ℃, and the sintering temperature of the existing formula is 1650 ℃; specifically, the preparation method of the silicon oxynitride ceramic lift tube provided by the invention adopts low liquid phase point material compatibility, so that low-temperature sintering of the silicon oxynitride ceramic is possible, and the sintering temperature of the existing formula is 1650 ℃ which is lower than the 1700 ℃ decomposition temperature of the silicon oxynitride material;
s6: processing and detecting: the burnt silicon oxynitride lift tube may have a certain dimensional deviation, and needs post-processing, specifically: adopting a grinder to process the burned silicon oxynitride lift tube to a designed size, and packaging and warehousing after the detection is qualified;
by adopting the preparation method of the silicon oxynitride ceramic lift tube, the strength of the prepared lift tube is higher (the breaking strength reaches about 400-500 megapascals), the thermal shock resistance is excellent, the oxidation resistance and the non-infiltration performance with aluminum liquid are obviously superior to those of the silicon nitride ceramic lift tube.
Preferably, in combination with the above scheme, the step S4 further includes isostatic pressing forming and lathe working:
s41: placing the homogenized ceramic powder into an isostatic pressing die, sealing and fastening by using rubber bands, and placing into an isostatic pressing machine;
s42: pressurizing to 300MPa, maintaining the pressure for 120 seconds, slowly releasing pressure, taking out the formed green compact, putting the green compact into a drying room at 50 ℃ for drying, simultaneously slowly releasing the stress of the ceramic green compact, putting the ceramic green compact for one week, and putting the ceramic green compact into a machining equipment machine tool for machining according to the design size.
Preferably, in combination with the above scheme, the pretreatment of lithium aluminate in S1 comprises: and (3) mixing the lithium carbonate and the aluminum hydroxide according to a preset molar ratio, respectively adding the mixture into a ball mill, ball milling the mixture with ethanol as a solvent, ball milling the mixture for 24 hours, discharging the mixture, drying the mixture, and calcining the mixture at 1250 ℃ for 6 hours to obtain the lithium aluminate block.
Preferably, in combination with the above scheme, in this embodiment, during the pretreatment of lithium aluminate: the preset molar ratio of the lithium carbonate to the aluminum hydroxide is 1:1, 1:2 and 1:3; crushing the burned lithium aluminate blocks into particles with the diameter of less than 1 mm, mixing the particles with ethanol, ball-grinding the particles into slurry with the diameter of less than 1 micron, drying, pulverizing, and packaging and marking; specifically, a plurality of groups of preset molar ratios of lithium carbonate and aluminum hydroxide can be designed for comparison; wherein, the preset molar ratio of the lithium carbonate to the aluminum hydroxide is 1:1 and is marked as an A1 raw material, the preset molar ratio of the lithium carbonate to the aluminum hydroxide is 1:2 and is marked as an A2 raw material, and the preset molar ratio of the lithium carbonate to the aluminum hydroxide is 1:2 and is marked as an A3 raw material.
Preferably, in combination with the above scheme, two sets of examples are specifically designed based on the two labeled A1 raw materials, A2 raw materials:
embodiment one: 80-90 parts of silicon oxynitride powder, 1-3 parts of calcined alumina, 1 3-6 parts of lithium aluminate, 1-5 parts of sintering aid (containing ferric oxide, yttrium oxide, barium carbonate, zinc oxide and the like), 1 part of dispersing agent, 3 parts of binder PVB (calculated according to dry powder and prepared into 10% solution), 100-150 parts of ethanol, adding into a stirring mill according to the formula proportion, ball-milling for 24 hours, and grinding and aging after reaching the granularity control index; then, the operation is performed according to the steps S3 to S6.
Embodiment two: 80-90 parts of silicon oxynitride, 1-3 parts of calcined alumina, 2 2-5 parts of lithium aluminate, 1-5 parts of sintering aid (containing ferric oxide, yttrium oxide, barium carbonate, zinc oxide and the like), 1 part of dispersing agent, 3 parts of binder PVB (calculated according to dry powder and prepared into 10% solution), 100-150 parts of alcohol, adding stirring mill according to the formula proportion, ball milling for 24 hours, and grinding and aging after reaching the granularity control index; then, the operation is performed according to the steps S3 to S6.
Preferably, in combination with the above scheme, the proportion of the lithium aluminate in the step S1 is selected to be 3-6 parts or 2-5 parts, wherein the proportion of the lithium aluminate is selected to be 3-6 parts, and the proportion is selected to be an A1 component; the proportion of the lithium aluminate is selected to be 2-5 parts of A2 component forming products.
Preferably, in combination with the above, the dispersant is selected from ammonium polyacrylate 9300 and the binder is selected from PVB (i.e., polyvinyl alcohol Ding Quanzhi).
Preferably, in combination with the above, the sintering aid comprises iron oxide, yttrium oxide, barium carbonate, and zinc oxide.
Preferably, in combination with the scheme, the silicon oxynitride powder is self-propagating synthetic silicon oxynitride; the granularity D50 of the silicon oxynitride powder is less than 3 microns, the silicon oxynitride content is not less than 98 percent, and the silicon nitride content is not more than 2 percent; in the scheme, the silicon oxynitride lift tube is designed for the first time, the thermal expansion coefficient of the silicon oxynitride is half that of silicon nitride, the service life is more than two years, and the service life is more than three times that of the silicon nitride ceramic lift tube; the oxidation resistance of silicon oxynitride and the stripping performance of aluminum liquid are far superior to those of silicon nitride ceramic lift tubes; meanwhile, compared with a silicon nitride ceramic lift tube, the self-propagating powder is adopted, so that the ceramic manufacturing cost is reduced by more than 20%.
Preferably, in combination with the above, the calcined alumina is microcrystalline alumina calcined using a mineralizer, the calcination temperature being less than 1300 ℃; the alpha phase content of the microcrystalline alumina is not less than 98%; the primary crystal size of the microcrystalline alumina is lower than 100 nanometers; after the calcination and the pulverization, the grain size D50 of the microcrystalline alumina is controlled to be 0.3-0.6 microns of industrial-grade calcined alpha alumina so as to reduce the synthesis temperature of the silicon oxynitride ceramic as much as possible.
Preferably, by combining the scheme, the aluminum hydroxide is selected to be ultrafine powder with more than 1 ten thousand meshes, the aluminum oxide content is more than 64 percent, and the alkali content is less than 0.2 percent.
Preferably, in combination with the above scheme, the lithium carbonate is selected from chemically pure lithium carbonate; further, S1 also comprises mineralizer, wherein the mineralizer is selected from chemically pure kaolin, basic magnesium carbonate, ferric oxide, zinc oxide, barium carbonate, yttrium oxide, cerium oxide and lanthanum oxide; specifically, the granularity of the mineralizer is controlled below 1 micron, so that the forming strength of the silicon oxynitride lift tube is effectively improved.
According to the preparation method of the silicon oxynitride ceramic lift tube, the low liquid phase point materials are adopted for compatibility, the sintering temperature is 1650 ℃, and the problem of high-temperature decomposition of silicon oxynitride is effectively solved by optimizing a ball milling process, a forming process and a sintering process, so that the breaking strength of the lift tube reaches about 400-500 megapascals; the self-propagating powder is adopted, the self-propagating powder is stable in production and quality, the large-scale mass production of the silicon oxynitride ceramic lift tube is possible, and the requirements of the domestic ceramic lift tube can be completely met.
In the scheme, the silicon oxynitride ceramic has low thermal expansion coefficient, oxidation resistance and non-wetting property with aluminum liquid, is far superior to a silicon nitride ceramic lift tube, and has service life more than two years and more than twice that of the silicon nitride ceramic lift tube; meanwhile, the self-propagating powder is adopted, so that the self-propagating powder is stable in production and quality, and the large-scale mass production of the silicon oxynitride ceramic lift tube is possible.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Many possible variations and modifications of the disclosed technology can be made by anyone skilled in the art, or equivalent embodiments with equivalent variations can be made, without departing from the scope of the disclosed technology. Therefore, any modification, equivalent variation and modification of the above embodiments according to the technology of the present invention fall within the protection scope of the present invention.
Claims (10)
1. The preparation method of the silicon oxynitride ceramic lift tube is characterized by comprising the following steps of:
s1: the selecting ingredients comprise:
80-90 parts of silicon oxynitride powder;
1-3 parts of calcined alumina;
2-6 parts of lithium aluminate;
1-5 parts of sintering aid;
1 part of dispersing agent;
3 parts of binder PVB;
100-150 parts of ethanol;
s2: proportioning and ball milling: adding the silicon oxynitride powder, the calcined alumina, the lithium aluminate, the sintering aid, the dispersing agent, the binder PVB and the ethanol selected in the step S1 into a stirring mill, and ball-milling for 22-26 hours to prepare uniform ceramic slurry;
s3: spray pulverizing: ageing and defoaming the prepared ceramic slurry for 22 to 26 hours, and spray-drying the ceramic slurry by a spray-drying tower to prepare ceramic powder conforming to the granularity grading; the moisture of the ceramic powder is controlled below 1%;
s4: homogenizing ceramic powder: after the prepared ceramic powder is aged for more than 48 hours, homogenizing for 30 minutes by using a homogenizer, adding a molding additive, and sub-packaging for later use;
s5: sintering of ceramics: sintering the ceramic powder in the step S4 into a ceramic silicon oxynitride lift tube; slowly heating up at the speed of 50 ℃ per hour, slowing down the heating up speed to 40 to 48 ℃ per hour at 300 to 400 ℃ and preserving heat for 6 hours at 500 to 700 ℃, then continuously heating up to 1650 ℃, preserving heat for 3 hours, and naturally cooling to normal temperature;
s6: processing and detecting: and (3) processing the burned silicon oxynitride lift tube to a designed size by adopting a grinding machine, and packaging and warehousing after the detection is qualified.
2. The method for preparing a silicon oxynitride ceramic lift tube according to claim 1, wherein the step S4 further comprises isostatic pressing and lathe working:
s41: placing the homogenized ceramic powder into an isostatic pressing die, sealing and fastening by using rubber bands, and placing into an isostatic pressing machine;
s42: pressurizing to 300MPa, maintaining the pressure for 120 seconds, slowly releasing pressure, taking out the formed green body, putting the green body into a drying room at 50 ℃ for drying, putting the green body into a machining equipment machine tool for machining according to the design size after one week of standing.
3. The method for preparing a silicon oxynitride ceramic lift tube according to claim 1, wherein the lithium aluminate pretreatment in S1 comprises: and (3) mixing the lithium carbonate and the aluminum hydroxide according to a preset molar ratio, respectively adding the mixture into a ball mill, ball milling the mixture with ethanol as a solvent, ball milling the mixture for 24 hours, discharging the mixture, drying the mixture, and calcining the mixture at 1250 ℃ for 6 hours to obtain the lithium aluminate block.
4. The method for preparing a silicon oxynitride ceramic lift tube according to claim 2, wherein during the pretreatment of lithium aluminate: the preset molar ratio of the lithium carbonate to the aluminum hydroxide is 1:1, 1:2 and 1:3; crushing the burned lithium aluminate blocks into particles with the diameter of less than 1 mm, mixing the particles with ethanol, ball-grinding the particles into slurry with the diameter of less than 1 micron, drying, pulverizing, and packaging and marking; the preset molar ratio of the lithium carbonate to the aluminum hydroxide is 1:1 and is recorded as an A1 raw material, the preset molar ratio of the lithium carbonate to the aluminum hydroxide is 1:2 and is recorded as an A2 raw material, and the preset molar ratio of the lithium carbonate to the aluminum hydroxide is 1:2 and is recorded as an A3 raw material.
5. The method for preparing a silicon oxynitride ceramic lift tube according to claim 1, wherein the proportion of lithium aluminate in S1 is selected from 3-6 parts or 2-5 parts.
6. The method of preparing a silicon oxynitride ceramic lift tube of claim 1, wherein the sintering aid comprises iron oxide, yttrium oxide, barium carbonate, and zinc oxide.
7. The method for preparing a silicon oxynitride ceramic lift tube according to claim 1, characterized in that the silicon oxynitride powder is self-propagating synthetic silicon oxynitride; the granularity D50 of the silicon oxynitride powder is less than 3 microns, the silicon oxynitride content is not less than 98%, and the silicon nitride content is not more than 2%.
8. The method for preparing a silicon oxynitride ceramic riser tube according to claim 1, wherein the calcined alumina is microcrystalline alumina calcined using a mineralizer, and the calcination temperature is lower than 1300 ℃; the alpha phase content of the microcrystalline alumina is not less than 98%; the primary crystal size of the microcrystalline alumina is lower than 100 nanometers; after the calcination and the pulverization, the grain size D50 of the microcrystalline alumina is controlled to be 0.3-0.6 microns.
9. The method for preparing a silicon oxynitride ceramic lift tube according to claim 3, characterized in that the aluminum hydroxide is selected from ultrafine powder with more than 1 ten thousand meshes, the aluminum oxide content is more than 64%, and the alkali content is less than 0.2%.
10. The method for preparing a silicon oxynitride ceramic lift tube according to claim 1, wherein the lithium carbonate is chemically pure lithium carbonate; the S1 also comprises a mineralizer, wherein the mineralizer is selected from chemically pure kaolin, basic magnesium carbonate, ferric oxide, zinc oxide, barium carbonate, yttrium oxide, cerium oxide and lanthanum oxide; the granularity of the mineralizer is controlled below 1 micron; the dispersing agent is ammonium polyacrylate 9300; the binder is PVB.
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