CN107285763A - A kind of preparation method of compound zirconia HTHP atomizer - Google Patents

A kind of preparation method of compound zirconia HTHP atomizer Download PDF

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CN107285763A
CN107285763A CN201710592485.1A CN201710592485A CN107285763A CN 107285763 A CN107285763 A CN 107285763A CN 201710592485 A CN201710592485 A CN 201710592485A CN 107285763 A CN107285763 A CN 107285763A
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nozzle
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chloride
hthp
temperature
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CN107285763B (en
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甘学贤
冯立明
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Jiaozuo Vina Science And Technology Co Ltd
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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, is made nozzle green compact;(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

A kind of preparation method of compound zirconia HTHP atomizer
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, 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 high there is provided a kind of compound zirconia of service life length 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 oil glue are put into mixer, mixes 2-3 hours, 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, plus 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, is made mobility and the good slurry of plasticity and mist projection granulating, is made available for isostatic pressed Pelletizing;
(4)By step(3)Nozzle is made in gained pelletizing isostatic pressing under 100-180Mpa, Digit Control Machine Tool green machined Green compact;
(5)High-temperature calcination is carried out to nozzle green compact, described sintering curve is:- 600 DEG C of room temperature, uniform heating in 12-18 hours is de- Fat;600-1350 DEG C, 9-12 hours uniform heating crystal-phase transformations;1350-1725 DEG C, 12-18 hours uniform heating sintering, 1725 DEG C insulation 6-10 hour insulation crystal grain handle;1725- room temperatures, 50 hours cold true, and 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 be plasticizer 1788, defoamer be 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 completely, while there is good sintering character again, densification degree is fine, therefore gained for material crystalline Sintered body has good high-temperature behavior, high temperature abrasion resistance, anti-corrosion property at high temperature concurrently simultaneously;Fine grinding is eventually passed to add 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 oil glue are put into mixer, mixes 2-3 hours, 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, plus 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, is made mobility and the good slurry of plasticity and mist projection granulating, is made available for isostatic pressed Pelletizing;
(4)By step(3)Nozzle is made in gained pelletizing isostatic pressing under 100-180Mpa, Digit Control Machine Tool green machined Green compact;
(5)High-temperature calcination is carried out to nozzle green compact, described sintering curve is:- 600 DEG C of room temperature, uniform heating in 12-18 hours is de- Fat;600-1350 DEG C, 9-12 hours uniform heating crystal-phase transformations;1350-1725 DEG C, 12-18 hours uniform heating sintering, 1725 DEG C insulation 6-10 hour insulation crystal grain handle;1725- room temperatures, 50 hours cold true, and 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 be plasticizer 1788, 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 oil glue are put into mixer, mixes 2 hours, mixed material is placed in Melting charge is prepared in electric smelting in electric arc furnaces, electric smelting temperature is 2600 DEG C, time 100min, then melting charge is milled to Raymond mill 1.5 microns of the particle diameter in position;
(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 ball In grinding machine, wet ball grinding to average grain diameter is less than 0.6 μm, adds 0.5wt% dispersant and 2wt% plasticizer and 0.5wt% Defoamer, is made mobility and the good slurry of plasticity and mist projection granulating, and the pelletizing available for isostatic pressed is made;
(4)By step(3)Nozzle green compact are made in gained pelletizing isostatic pressing under 100Mpa, Digit Control Machine Tool green machined;
(5)High-temperature calcination is carried out to nozzle green compact, described sintering curve is:- 600 DEG C of room temperature, uniform heating degreasing in 12 hours; 600-1350 DEG C, 9 hours uniform heating crystal-phase transformations;1350-1725 DEG C, 12 hours uniform heating sintering, 1725 DEG C of insulations 6 are small The processing of Shi Baowen crystal grain;1725- room temperatures, 50 hours cold true, and 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 that 86kg, magnesia are that 2 kg, calcium oxide are that 1.3 kg, petroleum coke are 6 kg.
Basic zirconium chloride is that 65 kg, calcium chloride are that 8 kg, magnesium chloride are 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 be plasticizer 1788, 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 of times)5 times, 1550 DEG C of high speed hard alloy injection liquid wash away use time for 3.2h.
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 oil glue are put into mixer, mixes 2.1 hours, mixed material is put Melting charge is prepared in electric smelting in electric arc furnaces, and electric smelting temperature is 2620 DEG C, time 105min, then melting charge is milled to Raymond mill 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 ball In grinding machine, 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, is made mobility and the good slurry of plasticity and mist projection granulating, and making available for isostatic pressed is made Grain powder;
(4)By step(3)Nozzle green compact are made in gained pelletizing isostatic pressing under 110Mpa, Digit Control Machine Tool green machined;
(5)High-temperature calcination is carried out to nozzle green compact, described sintering curve is:- 600 DEG C of room temperature, uniform heating degreasing in 13 hours; 600-1350 DEG C, 9.5 hours uniform heating crystal-phase transformations;1350-1725 DEG C, 13 hours uniform heating sintering, 1725 DEG C of insulations Insulation crystal grain processing in 6.5 hours;1725- room temperatures, 50 hours cold true, and 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 that 88kg, magnesia are that 2.9 kg, calcium oxide are that 2.5 kg, petroleum coke are 7 kg.
Basic zirconium chloride is that 69 kg, calcium chloride are that 10 kg, magnesium chloride are 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 be plasticizer 1788, 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 of times)6 times, 1550 DEG C of high speed hard alloy injection liquid wash away use time for 3.5h.
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 oil glue are put into mixer, mixes 2.2 hours, mixed material is put Melting charge is prepared in electric smelting in electric arc furnaces, and electric smelting temperature is 2650 DEG C, time 110min, then melting charge is milled to Raymond mill 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 ball In grinding machine, wet ball grinding to average grain diameter is less than 0.6 μm, adds 0.6wt% dispersant and 2.4wt% plasticizer and 0.6wt% 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)Nozzle green compact are made in gained pelletizing isostatic pressing under 120Mpa, Digit Control Machine Tool green machined;
(5)High-temperature calcination is carried out to nozzle green compact, described sintering curve is:- 600 DEG C of room temperature, uniform heating in 13.5 hours is de- Fat;600-1350 DEG C, 9.8 hours uniform heating crystal-phase transformations;1350-1725 DEG C, 13.5 hours uniform heating sintering, 1725 DEG C Insulation insulation crystal grain processing in 6.8 hours;1725- room temperatures, 50 hours cold true, and 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 that 89kg, magnesia are that 3.35 kg, calcium oxide are that 3.0 kg, petroleum coke are 7.5 kg.
Basic zirconium chloride is that 71 kg, calcium chloride are that 12 kg, magnesium chloride are 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 be plasticizer 1788, 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 of times)6 times, 1550 DEG C of high speed hard alloy injection liquid wash away use time for 3.6h.
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 oil glue are put into mixer, mixes 2.3 hours, mixed material is put Melting charge is prepared in electric smelting in electric arc furnaces, and electric smelting temperature is 2680 DEG C, time 115min, then melting charge is milled to Raymond mill 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, is added In ball mill, wet ball grinding to average grain diameter be less than 0.6 μm, add 0.65wt% dispersant and 2.6wt% plasticizer and 0.65wt% defoamer, is made mobility and the good slurry of plasticity and mist projection granulating, and making available for isostatic pressed is made Grain powder;
(4)By step(3)Nozzle green compact are made in gained pelletizing isostatic pressing under 130Mpa, Digit Control Machine Tool green machined;
(5)High-temperature calcination is carried out to nozzle green compact, described sintering curve is:- 600 DEG C of room temperature, uniform heating degreasing in 14 hours; 600-1350 DEG C, 10 hours uniform heating crystal-phase transformations;1350-1725 DEG C, 14 hours uniform heating sintering, 1725 DEG C of insulations Insulation crystal grain processing in 7.0 hours;1725- room temperatures, 50 hours cold true, and 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 that 90kg, magnesia are that 3.8 kg, calcium oxide are that 3.5 kg, petroleum coke are 8.0 kg.
Basic zirconium chloride is that 73 kg, calcium chloride are that 15 kg, magnesium chloride are 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 be plasticizer 1788, 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 of times)6 times, 1550 DEG C of high speed hard alloy injection liquid wash away use time for 3.8h.
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 oil glue are put into mixer, mixes 2.4 hours, mixed material is put Melting charge is prepared in electric smelting in electric arc furnaces, and electric smelting temperature is 2700 DEG C, time 120min, then melting charge is milled to Raymond mill 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 ball In grinding machine, wet ball grinding to average grain diameter is less than 0.6 μm, adds 0.7wt% dispersant and 2.8wt% plasticizer and 0.7wt% 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)Nozzle green compact are made in gained pelletizing isostatic pressing under 135Mpa, Digit Control Machine Tool green machined;
(5)High-temperature calcination is carried out to nozzle green compact, described sintering curve is:- 600 DEG C of room temperature, uniform heating in 14.5 hours is de- Fat;600-1350 DEG C, 10.2 hours uniform heating crystal-phase transformations;1350-1725 DEG C, 14.5 hours uniform heating sintering, 1725 DEG C insulation 7.2 hours insulation crystal grain processing;1725- room temperatures, 50 hours cold true, and 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 that 91kg, magnesia are that 4.25 kg, calcium oxide are that 4.0 kg, petroleum coke are 8.5 kg.
Basic zirconium chloride is that 75 kg, calcium chloride are that 16 kg, magnesium chloride are 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 be plasticizer 1788, 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 of times)8 times, 1550 DEG C of high speed hard alloy injection liquid wash away use time for 4.2h.
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 oil glue are put into mixer, mixes 2.5 hours, mixed material is put Melting charge is prepared in electric smelting in electric arc furnaces, and electric smelting temperature is 2750 DEG C, time 130min, then melting charge is milled to Raymond mill 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, is added In ball mill, wet ball grinding to average grain diameter be less than 0.6 μm, add 0.75wt% dispersant and 3wt% plasticizer and 0.75wt% defoamer, is made mobility and the good slurry of plasticity and mist projection granulating, and making available for isostatic pressed is made Grain powder;
(4)By step(3)Nozzle green compact are made in gained pelletizing isostatic pressing under 140Mpa, Digit Control Machine Tool green machined;
(5)High-temperature calcination is carried out to nozzle green compact, described sintering curve is:- 600 DEG C of room temperature, uniform heating degreasing in 15 hours; 600-1350 DEG C, 10.5 hours uniform heating crystal-phase transformations;1350-1725 DEG C, 15 hours uniform heating sintering, 1725 DEG C of insulations 7.5 hour insulation crystal grain processing;1725- room temperatures, 50 hours cold true, and 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 that 92kg, magnesia are that 6.6 kg, calcium oxide are that 4.5 kg, petroleum coke are 9.0 kg.
Basic zirconium chloride is that 77 kg, calcium chloride are that 17 kg, magnesium chloride are 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 be plasticizer 1788, defoamer is tributyl phosphate.
The use 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 oil glue are put into mixer, mixes 2.6 hours, mixed material is put Melting charge is prepared in electric smelting in electric arc furnaces, and electric smelting temperature is 2800 DEG C, time 140min, then melting charge is milled to Raymond mill 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 ball In grinding machine, wet ball grinding to average grain diameter is less than 0.6 μm, adds 0.8wt% dispersant and 3.2wt% plasticizer and 0.8wt% 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)Nozzle green compact are made in gained pelletizing isostatic pressing under 145Mpa, Digit Control Machine Tool green machined;
(5)High-temperature calcination is carried out to nozzle green compact, described sintering curve is:- 600 DEG C of room temperature, uniform heating in 15.5 hours is de- Fat;600-1350 DEG C, 10.8 hours uniform heating crystal-phase transformations;1350-1725 DEG C, 15.5 hours uniform heating sintering, 1725 DEG C insulation 8 hours insulation crystal grain processing;1725- room temperatures, 50 hours cold true, and 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 that 93kg, magnesia are that 5.15 kg, calcium oxide are that 5.0kg, petroleum coke are 9.5 kg.
Basic zirconium chloride is that 79 kg, calcium chloride are that 18 kg, magnesium chloride are 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 be plasticizer 1788, defoamer is tributyl phosphate.
The use 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 oil glue are put into mixer, mixes 2.7 hours, mixed material is put Melting charge is prepared in electric smelting in electric arc furnaces, and electric smelting temperature is 2850 DEG C, time 150min, then melting charge is milled to Raymond mill 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, is added In ball mill, wet ball grinding to average grain diameter be less than 0.6 μm, add 0.85wt% dispersant and 3.4wt% plasticizer and 0.85wt% defoamer, is made mobility and the good slurry of plasticity and mist projection granulating, and making available for isostatic pressed is made Grain powder;
(4)By step(3)Nozzle green compact are made in gained pelletizing isostatic pressing under 150Mpa, Digit Control Machine Tool green machined;
(5)High-temperature calcination is carried out to nozzle green compact, described sintering curve is:- 600 DEG C of room temperature, uniform heating degreasing in 16 hours; 600-1350 DEG C, 11 hours uniform heating crystal-phase transformations;1350-1725 DEG C, 16 hours uniform heating sintering, 1725 DEG C of insulations Insulation crystal grain processing in 8.5 hours;1725- room temperatures, 50 hours cold true, and 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 that 94kg, magnesia are that 5.60kg, calcium oxide are that 5.5kg, petroleum coke are 10 kg.
Basic zirconium chloride is that 81 kg, calcium chloride are that 19 kg, magnesium chloride are 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 be plasticizer 1788, defoamer is tributyl phosphate.
The use 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 oil glue are put into mixer, mixes 2.8 hours, mixed material is put Melting charge is prepared in electric smelting in electric arc furnaces, and electric smelting temperature is 2900 DEG C, time 160min, then melting charge is milled to Raymond mill 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 ball In grinding machine, wet ball grinding to average grain diameter is less than 0.6 μm, adds 0.9wt% dispersant and 3.6wt% plasticizer and 0.9wt% 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)Nozzle green compact are made in gained pelletizing isostatic pressing under 160Mpa, Digit Control Machine Tool green machined;
(5)High-temperature calcination is carried out to nozzle green compact, described sintering curve is:- 600 DEG C of room temperature, uniform heating in 16.5 hours is de- Fat;600-1350 DEG C, 11.5 hours uniform heating crystal-phase transformations;1350-1725 DEG C, 16.5 hours uniform heating sintering, 1725 DEG C insulation 9 hours insulation crystal grain processing;1725- room temperatures, 50 hours cold true, and 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 that 95kg, magnesia are that 6.05kg, calcium oxide are that 6.0kg, petroleum coke are 10.5 kg.
Basic zirconium chloride is that 85 kg, calcium chloride are that 20kg, magnesium chloride are 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 be plasticizer 1788, defoamer is tributyl phosphate.
The use 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 oil glue are put into mixer, mixes 2.9 hours, mixed material is put Melting charge is prepared in electric smelting in electric arc furnaces, and electric smelting temperature is 2950 DEG C, time 170min, then melting charge is milled to Raymond mill 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, is added In ball mill, wet ball grinding to average grain diameter be less than 0.6 μm, add 0.95wt% dispersant and 3.8wt% plasticizer and 0.95wt% defoamer, is made mobility and the good slurry of plasticity and mist projection granulating, and making available for isostatic pressed is made Grain powder;
(4)By step(3)Nozzle green compact are made in gained pelletizing isostatic pressing under 170Mpa, Digit Control Machine Tool green machined;
(5)High-temperature calcination is carried out to nozzle green compact, described sintering curve is:- 600 DEG C of room temperature, uniform heating degreasing in 17 hours; 600-1350 DEG C, 11.8 hours uniform heating crystal-phase transformations;1350-1725 DEG C, 17 hours uniform heating sintering, 1725 DEG C of insulations Insulation crystal grain processing in 9.5 hours;1725- room temperatures, 50 hours cold true, and 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 that 96kg, magnesia are that 6.5kg, calcium oxide are that 6.5kg, petroleum coke are 6.5 kg.
Basic zirconium chloride is that 87kg, calcium chloride are that 22kg, magnesium chloride are 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 be plasticizer 1788, defoamer is tributyl phosphate.
The use 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 oil glue are put into mixer, mixes 3 hours, mixed material is placed in Melting charge is prepared in electric smelting in electric arc furnaces, electric smelting temperature is 3000 DEG C, time 180min, then melting charge is milled to Raymond mill 1.5 microns of the particle diameter in position;
(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 ball In grinding machine, wet ball grinding to average grain diameter is less than 0.6 μm, adds 1wt% dispersant and 4wt% plasticizer and 1wt% froth breaking Agent, is made mobility and the good slurry of plasticity and mist projection granulating, and the pelletizing available for isostatic pressed is made;
(4)By step(3)Nozzle green compact are made in gained pelletizing isostatic pressing under 180Mpa, Digit Control Machine Tool green machined;
(5)High-temperature calcination is carried out to nozzle green compact, described sintering curve is:- 600 DEG C of room temperature, uniform heating degreasing in 18 hours; 600-1350 DEG C, 12 hours uniform heating crystal-phase transformations;1350-1725 DEG C, 18 hours uniform heating sintering, 1725 DEG C of insulations 10 Hour insulation crystal grain processing;1725- room temperatures, 50 hours cold true, and 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 that 97kg, magnesia are that 7kg, calcium oxide are that 7kg, petroleum coke are 11 kg.
Basic zirconium chloride is that 89kg, calcium chloride are that 25kg, magnesium chloride are 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 be plasticizer 1788, defoamer is tributyl phosphate.
The use 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 of times)3 times, 1550 DEG C of high speed hard alloy injection liquid wash away use time for 0.5h.
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)

1. a kind of preparation method of compound zirconia HTHP atomizer, it is characterised in that:Comprise the following steps that:
(1)Zirconium silicate, magnesia, calcium oxide and oil glue are put into mixer, mixes 2-3 hours, 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, plus 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, is made mobility and the good slurry of plasticity and mist projection granulating, is made available for isostatic pressed Pelletizing;
(4)By step(3)Nozzle is made in gained pelletizing isostatic pressing under 100-180Mpa, Digit Control Machine Tool green machined Green compact;
(5)High-temperature calcination is carried out to nozzle green compact, described sintering curve is:- 600 DEG C of room temperature, uniform heating in 12-18 hours is de- Fat;600-1350 DEG C, 9-12 hours uniform heating crystal-phase transformations;1350-1725 DEG C, 12-18 hours uniform heating sintering, 1725 DEG C insulation 6-10 hour insulation crystal grain handle;1725- room temperatures, 50 hours cold true, and 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 be plasticizer 1788, defoamer is tributyl phosphate.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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