CN107285763B - A kind of preparation method of compound zirconia HTHP atomizer - Google Patents
A kind of preparation method of compound zirconia HTHP atomizer Download PDFInfo
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- CN107285763B CN107285763B CN201710592485.1A CN201710592485A CN107285763B CN 107285763 B CN107285763 B CN 107285763B CN 201710592485 A CN201710592485 A CN 201710592485A CN 107285763 B CN107285763 B CN 107285763B
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 150000001875 compounds Chemical class 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 59
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 58
- 238000002844 melting Methods 0.000 claims abstract description 44
- 230000008018 melting Effects 0.000 claims abstract description 44
- 239000002270 dispersing agent Substances 0.000 claims abstract description 43
- 239000004014 plasticizer Substances 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 34
- 238000003723 Smelting Methods 0.000 claims abstract description 30
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000292 calcium oxide Substances 0.000 claims abstract description 30
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 30
- 238000005245 sintering Methods 0.000 claims abstract description 30
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 29
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 29
- 239000001110 calcium chloride Substances 0.000 claims abstract description 29
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 29
- 239000013530 defoamer Substances 0.000 claims abstract description 29
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 29
- 239000011236 particulate material Substances 0.000 claims abstract description 29
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims abstract description 29
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000003595 mist Substances 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000000975 co-precipitation Methods 0.000 claims abstract description 15
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 15
- 239000010432 diamond Substances 0.000 claims abstract description 15
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 15
- 238000000462 isostatic pressing Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000009413 insulation Methods 0.000 claims description 38
- 239000002006 petroleum coke Substances 0.000 claims description 28
- 238000005453 pelletization Methods 0.000 claims description 21
- 238000000227 grinding Methods 0.000 claims description 15
- 230000009466 transformation Effects 0.000 claims description 15
- 239000000084 colloidal system Substances 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 14
- 238000010891 electric arc Methods 0.000 claims description 14
- 238000001556 precipitation Methods 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 14
- 239000002002 slurry Substances 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 14
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical group CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 abstract description 9
- 238000005299 abrasion Methods 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 238000000280 densification Methods 0.000 abstract description 2
- 238000000498 ball milling Methods 0.000 abstract 1
- 239000003292 glue Substances 0.000 abstract 1
- 239000003921 oil Substances 0.000 abstract 1
- 238000005238 degreasing Methods 0.000 description 13
- 230000035939 shock Effects 0.000 description 13
- 239000000956 alloy Substances 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 7
- 238000002347 injection Methods 0.000 description 6
- 239000007924 injection Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 238000011056 performance test Methods 0.000 description 5
- 230000003628 erosive effect Effects 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 229910001928 zirconium oxide Inorganic materials 0.000 description 2
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical group CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
The invention discloses a kind of preparation method of compound zirconia HTHP atomizer, comprise the following steps that：（1）Zirconium silicate, magnesia, calcium oxide and oil glue are put into mixer, mixed, then prepare melting charge；（2）Basic zirconium chloride, calcium chloride and magnesium chloride are put into reactor, saturation ammoniacal liquor is added and carries out coprecipitation reaction；（3）By melting charge and particulate material mixing and ball milling, dispersant, plasticizer and defoamer, mist projection granulating are added；（4）By step（3）Isostatic pressing, nozzle green compact are made；（5）High-temperature calcination is carried out to nozzle green compact；（6）Nozzle blank is ground to by size finished product compound zirconia nozzle up to standard using diamond abrasive tool.The technique that the present invention is combined using chemical method and electric smelting method powder, so that material crystalline is complete, there is good sintering character again simultaneously, densification degree is fine, therefore gained sintered body has good high-temperature behavior, high temperature abrasion resistance, anti-corrosion property at high temperature concurrently simultaneously.
Description
Technical field
The invention belongs to the preparing technical field of electrostatic atomization apparatus, and in particular to a kind of compound zirconia HTHP mist
Change the preparation method of nozzle.
Background technology
HTHP atomizer is the crucial fire resisting erosion resistance part for entering to be about to alloy melt high-pressure atomization, main
Be used for cemented carbide industry, high-quality Powder Metallurgy Industry, due to these use occasion operating mode very severes, erosion, abrasion,
High temperature, violent thermal shock, in general refractory part are difficult to bear this operating mode, therefore zirconium oxide HTHP atomizer turns into pass
Key key element.At present, domestic preferably zirconium oxide HTHP atomizer is mainly regular oxidation zirconium refractory product, and mostly according to
Rely import, and the service life of compound zirconia HTHP atomizer improves 1-2 times compared with imported material, has filled up domestic skill
Art blank.
The content of the invention
The purpose of the present invention, which is that, overcomes existing technical deficiency, there is provided a kind of compound zirconia of service life length is high
The preparation method of warm high pressure atomizing nozzle.
The purpose of the present invention is realized in the following manner：
A kind of preparation method of compound zirconia HTHP atomizer, is comprised the following steps that：
（1）Zirconium silicate, magnesia, calcium oxide and petroleum coke are put into mixer, 2-3 hours are mixed, by mixed thing
Material is placed in electric smelting in electric arc furnaces and prepares melting charge, and electric smelting temperature is 2600-3000 DEG C, time 100-180min, then will melting
Material is milled to 1.5 microns of median with Raymond mill；
（2）Basic zirconium chloride, calcium chloride and magnesium chloride are put into reactor, saturation ammoniacal liquor is added and carries out coprecipitation reaction,
Gained precipitation colloid calcines the particulate material for preparing chemical method by 800-1100 DEG C；
（3）By step（1）Melting charge and step after obtained mill（2）Obtained particulate material is by 8:2-9:1 ratio is mixed
Close, add in ball mill, wet ball grinding to average grain diameter is less than 0.6 μm, adds the increasing of 0.5-1wt% dispersant and 2-4wt%
Agent and 0.5-1wt% defoamer are moulded, mobility and the good slurry of plasticity and mist projection granulating is made, is made and can be used for etc.
The pelletizing of static pressure；
（4）By step（3）Gained pelletizing isostatic pressing under 100-180Mpa, Digit Control Machine Tool green machined, it is made
Nozzle green compact；
（5）High-temperature calcination is carried out to nozzle green compact, described sintering curve is：- 600 DEG C of room temperature, 12-18 hours uniformly rise
Warm degreasing；600-1350 DEG C, 9-12 hours uniformly heat up crystal-phase transformation；1350-1725 DEG C, the 12-18 hours uniform sintering that heats up,
1725 DEG C of insulation 6-10 hours are incubated crystal grain processing；1725- room temperatures, cool down within 50 hours, this process is uniform decrease in temperature, no insulation；
（6）Nozzle blank is ground to by size finished product compound zirconia nozzle up to standard using diamond abrasive tool.
The zirconium silicate is 86-97 parts, magnesia is 2-7 parts, calcium oxide is 1.3-7 parts, petroleum coke is 6-11 parts.
The basic zirconium chloride is 65-89 parts, calcium chloride is 8-25 parts, magnesium chloride is 2.5-13 parts.
The step（2）The addition of middle saturation ammoniacal liquor is the 3-15% of solid masses in reactor.
The step（3）In dispersant be dispersant 9400, plasticizer is plasticizer 1788, and defoamer is tricresyl phosphate fourth
Ester.
Relative to prior art, manufacture craft of the present invention is reliable, and cost of material is low；By in oxygen in special cermacis formula
Change and the appropriate stabilizer magnesium oxide for playing transformation toughening effect, calcium oxide are introduced in zirconium powder body；Using chemical method and electric smelting method powder
The technique being combined so that material crystalline is complete, while has good sintering character again, and densification degree is fine, therefore gained
Sintered body has good high-temperature behavior, high temperature abrasion resistance, anti-corrosion property at high temperature concurrently simultaneously；Finally add by fine grinding
Work, obtained compound zirconia nozzle temperature in use is high, wear-resistant, resistance to erosion, good corrosion resistance；Service life is compared with imported material
Improve 1-2 times.
Embodiment
Embodiment 1：
A kind of preparation method of compound zirconia HTHP atomizer, is comprised the following steps that：
（1）Zirconium silicate, magnesia, calcium oxide and petroleum coke are put into mixer, 2-3 hours are mixed, by mixed thing
Material is placed in electric smelting in electric arc furnaces and prepares melting charge, and electric smelting temperature is 2600-3000 DEG C, time 100-180min, then will melting
Material is milled to 1.5 microns of median with Raymond mill；
（2）Basic zirconium chloride, calcium chloride and magnesium chloride are put into reactor, saturation ammoniacal liquor is added and carries out coprecipitation reaction,
Gained precipitation colloid calcines the particulate material for preparing chemical method by 800-1100 DEG C；
（3）By step（1）Melting charge and step after obtained mill（2）Obtained particulate material is by 8:2-9:1 ratio is mixed
Close, add in ball mill, wet ball grinding to average grain diameter is less than 0.6 μm, adds the increasing of 0.5-1wt% dispersant and 2-4wt%
Agent and 0.5-1wt% defoamer are moulded, mobility and the good slurry of plasticity and mist projection granulating is made, is made and can be used for etc.
The pelletizing of static pressure；
（4）By step（3）Gained pelletizing isostatic pressing under 100-180Mpa, Digit Control Machine Tool green machined, it is made
Nozzle green compact；
（5）High-temperature calcination is carried out to nozzle green compact, described sintering curve is：- 600 DEG C of room temperature, 12-18 hours uniformly rise
Warm degreasing；600-1350 DEG C, 9-12 hours uniformly heat up crystal-phase transformation；1350-1725 DEG C, the 12-18 hours uniform sintering that heats up,
1725 DEG C of insulation 6-10 hours are incubated crystal grain processing；1725- room temperatures, cool down within 50 hours, this process is uniform decrease in temperature, no insulation；
（6）Nozzle blank is ground to by size finished product compound zirconia nozzle up to standard using diamond abrasive tool.
Zirconium silicate is 86-97 parts, magnesia is 2-7 parts, calcium oxide is 1.3-7 parts, petroleum coke is 6-11 parts.
Basic zirconium chloride is 65-89 parts, calcium chloride is 8-25 parts, magnesium chloride is 2.5-13 parts.
Step（2）The addition of middle saturation ammoniacal liquor is the 3-15% of solid masses in reactor.
Step（3）In dispersant be dispersant 9400, plasticizer is plasticizer 1788, and defoamer is tributyl phosphate.
Embodiment 2：
A kind of preparation method of compound zirconia HTHP atomizer, is comprised the following steps that：
（1）Zirconium silicate, magnesia, calcium oxide and petroleum coke are put into mixer, mixed 2 hours, by mixed material
It is placed in electric smelting in electric arc furnaces and prepares melting charge, electric smelting temperature is 2600 DEG C, time 100min, then melting charge is ground with Raymond mill
To 1.5 microns of median；
（2）Basic zirconium chloride, calcium chloride and magnesium chloride are put into reactor, saturation ammoniacal liquor is added and carries out coprecipitation reaction,
Gained precipitation colloid calcines the particulate material for preparing chemical method by 800 DEG C；
（3）By step（1）Melting charge and step after obtained mill（2）Obtained particulate material is by 8:2 ratio mixing, adds
Enter in ball mill, wet ball grinding to average grain diameter be less than 0.6 μm, add 0.5wt% dispersant and 2wt% plasticizer and
0.5wt% defoamer, mobility and the good slurry of plasticity and mist projection granulating is made, making available for isostatic pressed is made
Grain powder；
（4）By step（3）Gained pelletizing isostatic pressing under 100Mpa, Digit Control Machine Tool green machined, nozzle is made
Green compact；
（5）High-temperature calcination is carried out to nozzle green compact, described sintering curve is：- 600 DEG C of room temperature, uniformly heating in 12 hours
Degreasing；600-1350 DEG C, uniformly heat up crystal-phase transformation for 9 hours；1350-1725 DEG C, uniformly heat up sintering for 12 hours, 1725 DEG C of guarantors
Temperature insulation crystal grain processing in 6 hours；1725- room temperatures, cool down within 50 hours, this process is uniform decrease in temperature, no insulation；
（6）Nozzle blank is ground to by size finished product compound zirconia nozzle up to standard using diamond abrasive tool.
Zirconium silicate is 86kg, magnesia is 2 kg, calcium oxide is 1.3 kg, petroleum coke is 6 kg.
Basic zirconium chloride is 65 kg, calcium chloride is 8 kg, magnesium chloride is 2.5 kg.
Step（2）The addition of middle saturation ammoniacal liquor is 3% of solid masses in reactor.
Step（3）In dispersant be dispersant 9400, plasticizer is plasticizer 1788, and defoamer is tributyl phosphate.
Performance test results：Bulk density：5.38g/cm3, anti-thermal shock（1300 DEG C to room-temperature water bath, thermal shock is not burst repeatedly
Number）5 times, it is 3.2h that 1550 DEG C of high speed hard alloy injection liquid, which wash away usage time,.
Embodiment 3：
A kind of preparation method of compound zirconia HTHP atomizer, is comprised the following steps that：
（1）Zirconium silicate, magnesia, calcium oxide and petroleum coke are put into mixer, mixed 2.1 hours, by mixed thing
Material is placed in electric smelting in electric arc furnaces and prepares melting charge, and electric smelting temperature is 2620 DEG C, time 105min, then by melting charge Raymond mill
It is milled to 1.5 microns of median；
（2）Basic zirconium chloride, calcium chloride and magnesium chloride are put into reactor, saturation ammoniacal liquor is added and carries out coprecipitation reaction,
Gained precipitation colloid calcines the particulate material for preparing chemical method by 820 DEG C；
（3）By step（1）Melting charge and step after obtained mill（2）Obtained particulate material is by 9:2 ratio mixing, adds
Enter in ball mill, wet ball grinding to average grain diameter be less than 0.6 μm, add 0.55wt% dispersant and 2.2wt% plasticizer and
0.55wt% defoamer, mobility and the good slurry of plasticity and mist projection granulating is made, making available for isostatic pressed is made
Grain powder；
（4）By step（3）Gained pelletizing isostatic pressing under 110Mpa, Digit Control Machine Tool green machined, nozzle is made
Green compact；
（5）High-temperature calcination is carried out to nozzle green compact, described sintering curve is：- 600 DEG C of room temperature, uniformly heating in 13 hours
Degreasing；600-1350 DEG C, uniformly heat up crystal-phase transformation for 9.5 hours；1350-1725 DEG C, uniformly heat up sintering for 13 hours, 1725 DEG C
Insulation insulation crystal grain processing in 6.5 hours；1725- room temperatures, cool down within 50 hours, this process is uniform decrease in temperature, no insulation；
（6）Nozzle blank is ground to by size finished product compound zirconia nozzle up to standard using diamond abrasive tool.
Zirconium silicate is 88kg, magnesia is 2.9 kg, calcium oxide is 2.5 kg, petroleum coke is 7 kg.
Basic zirconium chloride is 69 kg, calcium chloride is 10 kg, magnesium chloride is 4 kg.
Step（2）The addition of middle saturation ammoniacal liquor is 5% of solid masses in reactor.
Step（3）In dispersant be dispersant 9400, plasticizer is plasticizer 1788, and defoamer is tributyl phosphate.
Performance test results：Bulk density：5.35g/cm3, anti-thermal shock（1300 DEG C to room-temperature water bath, thermal shock is not burst repeatedly
Number）6 times, it is 3.5h that 1550 DEG C of high speed hard alloy injection liquid, which wash away usage time,.
Embodiment 4：
A kind of preparation method of compound zirconia HTHP atomizer, is comprised the following steps that：
（1）Zirconium silicate, magnesia, calcium oxide and petroleum coke are put into mixer, mixed 2.2 hours, by mixed thing
Material is placed in electric smelting in electric arc furnaces and prepares melting charge, and electric smelting temperature is 2650 DEG C, time 110min, then by melting charge Raymond mill
It is milled to 1.5 microns of median；
（2）Basic zirconium chloride, calcium chloride and magnesium chloride are put into reactor, saturation ammoniacal liquor is added and carries out coprecipitation reaction,
Gained precipitation colloid calcines the particulate material for preparing chemical method by 850 DEG C；
（3）By step（1）Melting charge and step after obtained mill（2）Obtained particulate material is by 5:1 ratio mixing, adds
Enter in ball mill, wet ball grinding to average grain diameter be less than 0.6 μm, add 0.6wt% dispersant and 2.4wt% plasticizer and
0.6wt% defoamer, mobility and the good slurry of plasticity and mist projection granulating is made, making available for isostatic pressed is made
Grain powder；
（4）By step（3）Gained pelletizing isostatic pressing under 120Mpa, Digit Control Machine Tool green machined, nozzle is made
Green compact；
（5）High-temperature calcination is carried out to nozzle green compact, described sintering curve is：- 600 DEG C of room temperature, uniformly rise within 13.5 hours
Warm degreasing；600-1350 DEG C, uniformly heat up crystal-phase transformation for 9.8 hours；1350-1725 DEG C, uniformly heat up sintering for 13.5 hours,
1725 DEG C of insulations insulation crystal grain processing in 6.8 hours；1725- room temperatures, cool down within 50 hours, this process is uniform decrease in temperature, no insulation；
（6）Nozzle blank is ground to by size finished product compound zirconia nozzle up to standard using diamond abrasive tool.
Zirconium silicate is 89kg, magnesia is 3.35 kg, calcium oxide is 3.0 kg, petroleum coke is 7.5 kg.
Basic zirconium chloride is 71 kg, calcium chloride is 12 kg, magnesium chloride is 5 kg.
Step（2）The addition of middle saturation ammoniacal liquor is 6% of solid masses in reactor.
Step（3）In dispersant be dispersant 9400, plasticizer is plasticizer 1788, and defoamer is tributyl phosphate.
Performance test results：Bulk density：5.33g/cm3, anti-thermal shock（1300 DEG C to room-temperature water bath, thermal shock is not burst repeatedly
Number）6 times, it is 3.6h that 1550 DEG C of high speed hard alloy injection liquid, which wash away usage time,.
Embodiment 5：
A kind of preparation method of compound zirconia HTHP atomizer, is comprised the following steps that：
（1）Zirconium silicate, magnesia, calcium oxide and petroleum coke are put into mixer, mixed 2.3 hours, by mixed thing
Material is placed in electric smelting in electric arc furnaces and prepares melting charge, and electric smelting temperature is 2680 DEG C, time 115min, then by melting charge Raymond mill
It is milled to 1.5 microns of median；
（2）Basic zirconium chloride, calcium chloride and magnesium chloride are put into reactor, saturation ammoniacal liquor is added and carries out coprecipitation reaction,
Gained precipitation colloid calcines the particulate material for preparing chemical method by 880 DEG C；
（3）By step（1）Melting charge and step after obtained mill（2）Obtained particulate material is by 11:2 ratio mixing,
Add in ball mill, wet ball grinding to average grain diameter is less than 0.6 μm, adds 0.65wt% dispersant and 2.6wt% plasticizer
With 0.65wt% defoamer, mobility and the good slurry of plasticity and mist projection granulating is made, is made available for isostatic pressed
Pelletizing；
（4）By step（3）Gained pelletizing isostatic pressing under 130Mpa, Digit Control Machine Tool green machined, nozzle is made
Green compact；
（5）High-temperature calcination is carried out to nozzle green compact, described sintering curve is：- 600 DEG C of room temperature, uniformly heating in 14 hours
Degreasing；600-1350 DEG C, uniformly heat up crystal-phase transformation for 10 hours；1350-1725 DEG C, uniformly heat up sintering for 14 hours, 1725 DEG C
Insulation insulation crystal grain processing in 7.0 hours；1725- room temperatures, cool down within 50 hours, this process is uniform decrease in temperature, no insulation；
（6）Nozzle blank is ground to by size finished product compound zirconia nozzle up to standard using diamond abrasive tool.
Zirconium silicate is 90kg, magnesia is 3.8 kg, calcium oxide is 3.5 kg, petroleum coke is 8.0 kg.
Basic zirconium chloride is 73 kg, calcium chloride is 15 kg, magnesium chloride is 6 kg.
Step（2）The addition of middle saturation ammoniacal liquor is 7% of solid masses in reactor.
Step（3）In dispersant be dispersant 9400, plasticizer is plasticizer 1788, and defoamer is tributyl phosphate.
Performance test results：Bulk density：5.31g/cm3, anti-thermal shock（1300 DEG C to room-temperature water bath, thermal shock is not burst repeatedly
Number）6 times, it is 3.8h that 1550 DEG C of high speed hard alloy injection liquid, which wash away usage time,.
Embodiment 6：
A kind of preparation method of compound zirconia HTHP atomizer, is comprised the following steps that：
（1）Zirconium silicate, magnesia, calcium oxide and petroleum coke are put into mixer, mixed 2.4 hours, by mixed thing
Material is placed in electric smelting in electric arc furnaces and prepares melting charge, and electric smelting temperature is 2700 DEG C, time 120min, then by melting charge Raymond mill
It is milled to 1.5 microns of median；
（2）Basic zirconium chloride, calcium chloride and magnesium chloride are put into reactor, saturation ammoniacal liquor is added and carries out coprecipitation reaction,
Gained precipitation colloid calcines the particulate material for preparing chemical method by 900 DEG C；
（3）By step（1）Melting charge and step after obtained mill（2）Obtained particulate material is by 6:1 ratio mixing, adds
Enter in ball mill, wet ball grinding to average grain diameter be less than 0.6 μm, add 0.7wt% dispersant and 2.8wt% plasticizer and
0.7wt% defoamer, mobility and the good slurry of plasticity and mist projection granulating is made, making available for isostatic pressed is made
Grain powder；
（4）By step（3）Gained pelletizing isostatic pressing under 135Mpa, Digit Control Machine Tool green machined, nozzle is made
Green compact；
（5）High-temperature calcination is carried out to nozzle green compact, described sintering curve is：- 600 DEG C of room temperature, uniformly rise within 14.5 hours
Warm degreasing；600-1350 DEG C, uniformly heat up crystal-phase transformation for 10.2 hours；1350-1725 DEG C, uniformly heat up sintering for 14.5 hours,
1725 DEG C of insulations insulation crystal grain processing in 7.2 hours；1725- room temperatures, cool down within 50 hours, this process is uniform decrease in temperature, no insulation；
（6）Nozzle blank is ground to by size finished product compound zirconia nozzle up to standard using diamond abrasive tool.
Zirconium silicate is 91kg, magnesia is 4.25 kg, calcium oxide is 4.0 kg, petroleum coke is 8.5 kg.
Basic zirconium chloride is 75 kg, calcium chloride is 16 kg, magnesium chloride 7kg.
Step（2）The addition of middle saturation ammoniacal liquor is 8% of solid masses in reactor.
Step（3）In dispersant be dispersant 9400, plasticizer is plasticizer 1788, and defoamer is tributyl phosphate.
Performance test results：Bulk density：5.28g/cm3, anti-thermal shock（1300 DEG C to room-temperature water bath, thermal shock is not burst repeatedly
Number）8 times, it is 4.2h that 1550 DEG C of high speed hard alloy injection liquid, which wash away usage time,.
Embodiment 7：
A kind of preparation method of compound zirconia HTHP atomizer, is comprised the following steps that：
（1）Zirconium silicate, magnesia, calcium oxide and petroleum coke are put into mixer, mixed 2.5 hours, by mixed thing
Material is placed in electric smelting in electric arc furnaces and prepares melting charge, and electric smelting temperature is 2750 DEG C, time 130min, then by melting charge Raymond mill
It is milled to 1.5 microns of median；
（2）Basic zirconium chloride, calcium chloride and magnesium chloride are put into reactor, saturation ammoniacal liquor is added and carries out coprecipitation reaction,
Gained precipitation colloid calcines the particulate material for preparing chemical method by 920 DEG C；
（3）By step（1）Melting charge and step after obtained mill（2）Obtained particulate material is by 13:2 ratio mixing,
Add ball mill in, wet ball grinding to average grain diameter be less than 0.6 μm, add 0.75wt% dispersant and 3wt% plasticizer and
0.75wt% defoamer, mobility and the good slurry of plasticity and mist projection granulating is made, making available for isostatic pressed is made
Grain powder；
（4）By step（3）Gained pelletizing isostatic pressing under 140Mpa, Digit Control Machine Tool green machined, nozzle is made
Green compact；
（5）High-temperature calcination is carried out to nozzle green compact, described sintering curve is：- 600 DEG C of room temperature, uniformly heating in 15 hours
Degreasing；600-1350 DEG C, uniformly heat up crystal-phase transformation for 10.5 hours；1350-1725 DEG C, uniformly heat up sintering for 15 hours, and 1725
DEG C insulation 7.5 hours insulation crystal grain processing；1725- room temperatures, cool down within 50 hours, this process is uniform decrease in temperature, no insulation；
（6）Nozzle blank is ground to by size finished product compound zirconia nozzle up to standard using diamond abrasive tool.
Zirconium silicate is 92kg, magnesia is 6.6 kg, calcium oxide is 4.5 kg, petroleum coke is 9.0 kg.
Basic zirconium chloride is 77 kg, calcium chloride is 17 kg, magnesium chloride 8kg.
Step（2）The addition of middle saturation ammoniacal liquor is 9% of solid masses in reactor.
Step（3）In dispersant be dispersant 9400, plasticizer is plasticizer 1788, and defoamer is tributyl phosphate.
The usage time for the atomizer that the present embodiment is produced is 4.3h.
Embodiment 8：
A kind of preparation method of compound zirconia HTHP atomizer, is comprised the following steps that：
（1）Zirconium silicate, magnesia, calcium oxide and petroleum coke are put into mixer, mixed 2.6 hours, by mixed thing
Material is placed in electric smelting in electric arc furnaces and prepares melting charge, and electric smelting temperature is 2800 DEG C, time 140min, then by melting charge Raymond mill
It is milled to 1.5 microns of median；
（2）Basic zirconium chloride, calcium chloride and magnesium chloride are put into reactor, saturation ammoniacal liquor is added and carries out coprecipitation reaction,
Gained precipitation colloid calcines the particulate material for preparing chemical method by 950 DEG C；
（3）By step（1）Melting charge and step after obtained mill（2）Obtained particulate material is by 7:1 ratio mixing, adds
Enter in ball mill, wet ball grinding to average grain diameter be less than 0.6 μm, add 0.8wt% dispersant and 3.2wt% plasticizer and
0.8wt% defoamer, mobility and the good slurry of plasticity and mist projection granulating is made, making available for isostatic pressed is made
Grain powder；
（4）By step（3）Gained pelletizing isostatic pressing under 145Mpa, Digit Control Machine Tool green machined, nozzle is made
Green compact；
（5）High-temperature calcination is carried out to nozzle green compact, described sintering curve is：- 600 DEG C of room temperature, uniformly rise within 15.5 hours
Warm degreasing；600-1350 DEG C, uniformly heat up crystal-phase transformation for 10.8 hours；1350-1725 DEG C, uniformly heat up sintering for 15.5 hours,
1725 DEG C of insulations insulation crystal grain processing in 8 hours；1725- room temperatures, cool down within 50 hours, this process is uniform decrease in temperature, no insulation；
（6）Nozzle blank is ground to by size finished product compound zirconia nozzle up to standard using diamond abrasive tool.
Zirconium silicate is 93kg, magnesia is 5.15 kg, calcium oxide 5.0kg, petroleum coke are 9.5 kg.
Basic zirconium chloride is 79 kg, calcium chloride is 18 kg, magnesium chloride 9kg.
Step（2）The addition of middle saturation ammoniacal liquor is 10% of solid masses in reactor.
Step（3）In dispersant be dispersant 9400, plasticizer is plasticizer 1788, and defoamer is tributyl phosphate.
The usage time for the atomizer that the present embodiment is produced is 3.9h.
Embodiment 9：
A kind of preparation method of compound zirconia HTHP atomizer, is comprised the following steps that：
（1）Zirconium silicate, magnesia, calcium oxide and petroleum coke are put into mixer, mixed 2.7 hours, by mixed thing
Material is placed in electric smelting in electric arc furnaces and prepares melting charge, and electric smelting temperature is 2850 DEG C, time 150min, then by melting charge Raymond mill
It is milled to 1.5 microns of median；
（2）Basic zirconium chloride, calcium chloride and magnesium chloride are put into reactor, saturation ammoniacal liquor is added and carries out coprecipitation reaction,
Gained precipitation colloid calcines the particulate material for preparing chemical method by 1000 DEG C；
（3）By step（1）Melting charge and step after obtained mill（2）Obtained particulate material is by 15:2 ratio mixing,
Add in ball mill, wet ball grinding to average grain diameter is less than 0.6 μm, adds 0.85wt% dispersant and 3.4wt% plasticizer
With 0.85wt% defoamer, mobility and the good slurry of plasticity and mist projection granulating is made, is made available for isostatic pressed
Pelletizing；
（4）By step（3）Gained pelletizing isostatic pressing under 150Mpa, Digit Control Machine Tool green machined, nozzle is made
Green compact；
（5）High-temperature calcination is carried out to nozzle green compact, described sintering curve is：- 600 DEG C of room temperature, uniformly heating in 16 hours
Degreasing；600-1350 DEG C, uniformly heat up crystal-phase transformation for 11 hours；1350-1725 DEG C, uniformly heat up sintering for 16 hours, 1725 DEG C
Insulation insulation crystal grain processing in 8.5 hours；1725- room temperatures, cool down within 50 hours, this process is uniform decrease in temperature, no insulation；
（6）Nozzle blank is ground to by size finished product compound zirconia nozzle up to standard using diamond abrasive tool.
Zirconium silicate is 94kg, magnesia 5.60kg, calcium oxide 5.5kg, petroleum coke are 10 kg.
Basic zirconium chloride is 81 kg, calcium chloride is 19 kg, magnesium chloride 10kg.
Step（2）The addition of middle saturation ammoniacal liquor is 12% of solid masses in reactor.
Step（3）In dispersant be dispersant 9400, plasticizer is plasticizer 1788, and defoamer is tributyl phosphate.
The usage time for the atomizer that the present embodiment is produced is 3.7h.
Embodiment 10：
A kind of preparation method of compound zirconia HTHP atomizer, is comprised the following steps that：
（1）Zirconium silicate, magnesia, calcium oxide and petroleum coke are put into mixer, mixed 2.8 hours, by mixed thing
Material is placed in electric smelting in electric arc furnaces and prepares melting charge, and electric smelting temperature is 2900 DEG C, time 160min, then by melting charge Raymond mill
It is milled to 1.5 microns of median；
（2）Basic zirconium chloride, calcium chloride and magnesium chloride are put into reactor, saturation ammoniacal liquor is added and carries out coprecipitation reaction,
Gained precipitation colloid calcines the particulate material for preparing chemical method by 1020 DEG C；
（3）By step（1）Melting charge and step after obtained mill（2）Obtained particulate material is by 8:1 ratio mixing, adds
Enter in ball mill, wet ball grinding to average grain diameter be less than 0.6 μm, add 0.9wt% dispersant and 3.6wt% plasticizer and
0.9wt% defoamer, mobility and the good slurry of plasticity and mist projection granulating is made, making available for isostatic pressed is made
Grain powder；
（4）By step（3）Gained pelletizing isostatic pressing under 160Mpa, Digit Control Machine Tool green machined, nozzle is made
Green compact；
（5）High-temperature calcination is carried out to nozzle green compact, described sintering curve is：- 600 DEG C of room temperature, uniformly rise within 16.5 hours
Warm degreasing；600-1350 DEG C, uniformly heat up crystal-phase transformation for 11.5 hours；1350-1725 DEG C, uniformly heat up sintering for 16.5 hours,
1725 DEG C of insulations insulation crystal grain processing in 9 hours；1725- room temperatures, cool down within 50 hours, this process is uniform decrease in temperature, no insulation；
（6）Nozzle blank is ground to by size finished product compound zirconia nozzle up to standard using diamond abrasive tool.
Zirconium silicate is 95kg, magnesia 6.05kg, calcium oxide 6.0kg, petroleum coke are 10.5 kg.
Basic zirconium chloride is 85 kg, calcium chloride 20kg, magnesium chloride 11kg.
Step（2）The addition of middle saturation ammoniacal liquor is 13% of solid masses in reactor.
Step（3）In dispersant be dispersant 9400, plasticizer is plasticizer 1788, and defoamer is tributyl phosphate.
The usage time for the atomizer that the present embodiment is produced is 3.7h.
Embodiment 11：
A kind of preparation method of compound zirconia HTHP atomizer, is comprised the following steps that：
（1）Zirconium silicate, magnesia, calcium oxide and petroleum coke are put into mixer, mixed 2.9 hours, by mixed thing
Material is placed in electric smelting in electric arc furnaces and prepares melting charge, and electric smelting temperature is 2950 DEG C, time 170min, then by melting charge Raymond mill
It is milled to 1.5 microns of median；
（2）Basic zirconium chloride, calcium chloride and magnesium chloride are put into reactor, saturation ammoniacal liquor is added and carries out coprecipitation reaction,
Gained precipitation colloid calcines the particulate material for preparing chemical method by 1050 DEG C；
（3）By step（1）Melting charge and step after obtained mill（2）Obtained particulate material is by 17:2 ratio mixing,
Add in ball mill, wet ball grinding to average grain diameter is less than 0.6 μm, adds 0.95wt% dispersant and 3.8wt% plasticizer
With 0.95wt% defoamer, mobility and the good slurry of plasticity and mist projection granulating is made, is made available for isostatic pressed
Pelletizing；
（4）By step（3）Gained pelletizing isostatic pressing under 170Mpa, Digit Control Machine Tool green machined, nozzle is made
Green compact；
（5）High-temperature calcination is carried out to nozzle green compact, described sintering curve is：- 600 DEG C of room temperature, uniformly heating in 17 hours
Degreasing；600-1350 DEG C, uniformly heat up crystal-phase transformation for 11.8 hours；1350-1725 DEG C, uniformly heat up sintering for 17 hours, and 1725
DEG C insulation 9.5 hours insulation crystal grain processing；1725- room temperatures, cool down within 50 hours, this process is uniform decrease in temperature, no insulation；
（6）Nozzle blank is ground to by size finished product compound zirconia nozzle up to standard using diamond abrasive tool.
Zirconium silicate is 96kg, magnesia 6.5kg, calcium oxide 6.5kg, petroleum coke are 6.5 kg.
Basic zirconium chloride is 87kg, calcium chloride 22kg, magnesium chloride 12kg.
Step（2）The addition of middle saturation ammoniacal liquor is 14% of solid masses in reactor.
Step（3）In dispersant be dispersant 9400, plasticizer is plasticizer 1788, and defoamer is tributyl phosphate.
The usage time for the atomizer that the present embodiment is produced is 3.5h.
Embodiment 12：
A kind of preparation method of compound zirconia HTHP atomizer, is comprised the following steps that：
（1）Zirconium silicate, magnesia, calcium oxide and petroleum coke are put into mixer, mixed 3 hours, by mixed material
It is placed in electric smelting in electric arc furnaces and prepares melting charge, electric smelting temperature is 3000 DEG C, time 180min, then melting charge is ground with Raymond mill
To 1.5 microns of median；
（2）Basic zirconium chloride, calcium chloride and magnesium chloride are put into reactor, saturation ammoniacal liquor is added and carries out coprecipitation reaction,
Gained precipitation colloid calcines the particulate material for preparing chemical method by 1100 DEG C；
（3）By step（1）Melting charge and step after obtained mill（2）Obtained particulate material is by 9:1 ratio mixing, adds
Enter in ball mill, wet ball grinding to average grain diameter is less than 0.6 μm, adds 1wt% dispersant and 4wt% plasticizer and 1wt%
Defoamer, mobility and the good slurry of plasticity and mist projection granulating is made, the pelletizing available for isostatic pressed is made；
（4）By step（3）Gained pelletizing isostatic pressing under 180Mpa, Digit Control Machine Tool green machined, nozzle is made
Green compact；
（5）High-temperature calcination is carried out to nozzle green compact, described sintering curve is：- 600 DEG C of room temperature, uniformly heating in 18 hours
Degreasing；600-1350 DEG C, uniformly heat up crystal-phase transformation for 12 hours；1350-1725 DEG C, uniformly heat up sintering for 18 hours, 1725 DEG C
Insulation insulation crystal grain processing in 10 hours；1725- room temperatures, cool down within 50 hours, this process is uniform decrease in temperature, no insulation；
（6）Nozzle blank is ground to by size finished product compound zirconia nozzle up to standard using diamond abrasive tool.
Zirconium silicate is 97kg, magnesia 7kg, calcium oxide 7kg, petroleum coke are 11 kg.
Basic zirconium chloride is 89kg, calcium chloride 25kg, magnesium chloride 13kg.
Step（2）The addition of middle saturation ammoniacal liquor is 15% of solid masses in reactor.
Step（3）In dispersant be dispersant 9400, plasticizer is plasticizer 1788, and defoamer is tributyl phosphate.
The usage time for the atomizer that the present embodiment is produced is 3.3h.
Conventional products performance：Bulk density：4.8g/cm3, anti-thermal shock（1300 DEG C to room-temperature water bath, thermal shock is not burst repeatedly
Number）3 times, it is 0.5h that 1550 DEG C of high speed hard alloy injection liquid, which wash away usage time,.
Above-described is only the preferred embodiment of the present invention, it is noted that for those skilled in the art,
Under the premise of general idea of the present invention is not departed from, some changes and improvements can also be made, these should also be considered as the present invention's
Protection domain.
Claims (5)
- A kind of 1. preparation method of compound zirconia HTHP atomizer, it is characterised in that：Comprise the following steps that：（1）Zirconium silicate, magnesia, calcium oxide and petroleum coke are put into mixer, 2-3 hours is mixed, mixed material is put Melting charge is prepared in electric smelting in electric arc furnaces, and electric smelting temperature is 2600-3000 DEG C, time 100-180min, then melting charge is used Raymond mill is milled to 1.5 microns of median；（2）Basic zirconium chloride, calcium chloride and magnesium chloride are put into reactor, saturation ammoniacal liquor is added and carries out coprecipitation reaction, gained Precipitation colloid calcines the particulate material for preparing chemical method by 800-1100 DEG C；（3）By step（1）Melting charge and step after obtained mill（2）Obtained particulate material is by 8:2-9:1 ratio mixing, adds Enter in ball mill, wet ball grinding to average grain diameter be less than 0.6 μm, add 0.5-1wt% dispersant and 2-4wt% plasticizer and 0.5-1wt% defoamer, mobility and the good slurry of plasticity and mist projection granulating is made, is made available for isostatic pressed Pelletizing；（4）By step（3）Gained pelletizing isostatic pressing under 100-180Mpa, Digit Control Machine Tool green machined, nozzle is made Green compact；（5）High-temperature calcination is carried out to nozzle green compact, described sintering curve is：- 600 DEG C of room temperature, 12-18 hours, uniformly heating was de- Fat；600-1350 DEG C, 9-12 hours uniformly heat up crystal-phase transformation；1350-1725 DEG C, the 12-18 hours uniform sintering that heats up, 1725 DEG C insulation 6-10 hours be incubated crystal grain handle；1725 DEG C-room temperature, cool down within 50 hours, this process is uniform decrease in temperature, no insulation；（6）Nozzle blank is ground to by size finished product compound zirconia nozzle up to standard using diamond abrasive tool.
- 2. the preparation method of compound zirconia HTHP atomizer according to claim 1, it is characterised in that：It is described Zirconium silicate is 86-97 parts, magnesia is 2-7 parts, calcium oxide is 1.3-7 parts, petroleum coke is 6-11 parts.
- 3. the preparation method of compound zirconia HTHP atomizer according to claim 1, it is characterised in that：It is described Basic zirconium chloride is 65-89 parts, calcium chloride is 8-25 parts, magnesium chloride is 2.5-13 parts.
- 4. the preparation method of compound zirconia HTHP atomizer according to claim 1, it is characterised in that：It is described Step（2）The addition of middle saturation ammoniacal liquor is the 3-15% of solid masses in reactor.
- 5. the preparation method of compound zirconia HTHP atomizer according to claim 1, it is characterised in that：It is described Step（3）In dispersant be dispersant 9400, plasticizer is plasticizer 1788, and defoamer is tributyl phosphate.
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| CN101289320A (en) * | 2008-05-21 | 2008-10-22 | 华南理工大学 | Process for preparing punching die by using ZTA material |
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| CN102653417A (en) * | 2012-03-26 | 2012-09-05 | 三祥新材股份有限公司 | Method for preparing stable-type zirconium dioxide by electric smelting method |
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| CN101074116A (en) * | 2007-06-27 | 2007-11-21 | 仙桃市中星电子材料有限公司 | Production of superfine mono-dispered nano-zirconium dioxide |
| CN101289320A (en) * | 2008-05-21 | 2008-10-22 | 华南理工大学 | Process for preparing punching die by using ZTA material |
| CN102060530A (en) * | 2010-11-16 | 2011-05-18 | 上海材料研究所 | Preparation method of compact zirconia ceramic plunger |
| CN102653417A (en) * | 2012-03-26 | 2012-09-05 | 三祥新材股份有限公司 | Method for preparing stable-type zirconium dioxide by electric smelting method |
| CN102976762A (en) * | 2012-11-07 | 2013-03-20 | 洛阳北苑特种陶瓷有限公司 | Method for preparing zirconia ceramic product |
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