Preparation process of efficient tungsten alloy heater

Abstract

The invention relates to the technical field of heaters, and discloses a preparation process of an efficient tungsten alloy heater. Comprising the following steps: S1, mixing a zirconium oxide composition and aluminum oxide according to a mass ratio of (20-26): (74-80), and carrying out compression molding to obtain an aluminum oxide blank; s2, a piece of aluminum oxide blank is taken, tungsten alloy heating conductive paste is printed, a heating wire is formed, then the aluminum oxide blank is covered, die-casting forming is conducted, and a tungsten alloy heater is obtained; the width of the aluminum oxide blank is 20-25 mm, the length of the aluminum oxide blank is 300 mm, and the thickness of the aluminum oxide blank is 1.15 mm; the width of the heating wire is 1.5 mm, and a 20mm non-heating area of the leading-out wire is reserved during printing. The zirconium oxide composition is prepared from zirconium oxide and a stabilizer in a mass ratio of (10-15): (85-90). The prepared tungsten alloy heater has good corrosion resistance and thermal shock resistance.

Description

TECHNICAL FIELD

[0001] The application relates to the technical field of a heater, and discloses a preparation process of a high-efficiency tungsten alloy heater. BACKGROUND

[0002] The tungsten alloy has the advantages of high strength and high temperature resistance, and can convert electric energy into heat energy after being electrified, and is commonly used as a heating slurry of a heater. However, the tungsten alloy heating slurry is prone to oxidation at high temperature, and therefore an aluminum oxide blank plate is commonly used as a protective layer to slow down the oxidation.

[0003] The aluminum oxide is an ideal heat-resistant material, but is prone to cracks during high-temperature operation due to insufficient toughness, thereby reducing the overall thermal shock resistance and corrosion resistance. The prior art commonly uses zirconium oxide to toughen the aluminum oxide. The zirconium oxide has different crystal forms in different temperature ranges, and is accompanied by volume expansion during phase transition, which causes some microcracks. Due to the offset effect of the microcracks, the toughness and the thermal shock resistance can be improved. However, if the introduction is improper, the cracks will be too large to affect the corrosion resistance and other performances. Therefore, it is of great significance to study how to prepare a high-efficiency tungsten alloy heater with both thermal shock resistance and corrosion resistance. SUMMARY

[0004] The application aims to provide a preparation process of a high-efficiency tungsten alloy heater to solve the problems in the background.

[0005] To solve the above technical problems, the application provides the following technical scheme: a preparation process of a high-efficiency tungsten alloy heater, comprising the following steps: S1: mixing a zirconium oxide composition and aluminum oxide according to a mass ratio of (20-26):(74-80) (the rotating speed is 20000r / min during mixing), and pressing forming to obtain aluminum oxide blank; S2: taking an aluminum oxide blank, printing a tungsten alloy heating and conducting slurry to form a heating wire, and then covering the aluminum oxide blank and pressure casting to obtain a tungsten alloy heater with a thickness of 1.5mm.

[0006] More preferably, the specification of the aluminum oxide blank is 20-25mm in width, 300mm in length, and 1.15mm in thickness; the heating wire is 1.5mm in width, and 20mm in non-heating area of the lead-out line is reserved during printing; the design heating temperature is 1500 DEG C, the working voltage is 660V, the working current is 1.31A, the resistance is 500Ω, the resistance per meter is 334Ω, and the length of the printed heating wire is 1500mm. Alumina has high melting point and high thermal stability, is an ideal heat-resistant material, but high temperature operation is prone to burst, so the prior art often introduces zirconium oxide ions into alumina. When the temperature changes, the crystal form of zirconium oxide changes, which is accompanied by volume expansion. Since it is only the volume expansion of small grains, it will not cause the entire material to crack, but only some micro-cracks will be generated around the grains. Due to the offset effect of these micro-cracks, the overall toughness and thermal shock resistance are improved.

[0007] More optimized, tungsten alloy heating conductive paste composition: composition 99.9W-0.06Ni-0.04Fe (mass percent); The tungsten alloy heating conductive paste is powered to raise the temperature to 600°C or more and 3410°C or less in 3 seconds. The heating temperature is controlled within 1100°C by adjusting the resistance of the heating circuit. High-temperature operation is prone to oxidation, so it needs to be compounded with alumina blank to increase the protective layer and isolate air to solve the oxidation problem.

[0008] More optimized, S1 step compression molding process: under the condition of 60~65℃, pressure 100~120MPa, static pressure 300~350s; S2 step compression molding process: 1600~1650℃, 1 ton under pressure casting.

[0009] More optimized, the zirconia combination is mass ratio (10~15): (85~90) of zirconia with particle size 1~2um and stabilizer. By controlling the amount of zirconia combination and the particle size of zirconia, it can not only ensure the necessary phase transition, but also avoid destructive volume expansion.

[0010] More optimized, the stabilizer includes yttria-stabilized zirconia with particle size 2~5um.

[0011] More optimized, the preparation of yttria-stabilized zirconia includes the following steps: adding zirconia, yttria, alumina, and dispersant ammonium polymethacrylate into water and stirring uniformly to obtain a slurry with a solid content of 50~55wt%, grinding, adding water again to adjust the solid content to 30~35wt%, grinding, spraying and drying, pre-burning at 700~900℃ for 2~3h, calcining at 1300~1400℃ for 3~4h, grinding and sieving to obtain yttria-stabilized zirconia with particle size 2~5um.

[0012] More optimized, the yttria-stabilized zirconia includes the following raw materials, by mass fraction: 94~95 parts of zirconia, 5~6 parts of yttria, 0.05~0.1 parts of alumina, and 0.01~0.02 parts of dispersant ammonium polymethacrylate.

[0013] The cation radius of yttria is close to that of Zr 4+ Dissolved in ZrO2, it plays the role of stabilizer.

[0014] More preferably, since yttrium is a rare earth element, it is relatively rare and expensive, so the composition of modified silicon carbide and silicon dioxide coated zirconium oxide is partially replaced; the stabilizer is yttria stabilized zirconia, silicon dioxide coated zirconia, and modified silicon carbide in a mass ratio of (1-2):(10-15):(0.5-0.8).

[0015] More preferably, the preparation of the silicon dioxide coated zirconia includes the following steps: taking an ethanol aqueous solution, zirconium oxide, and cetyltrimethylammonium bromide, ultrasonic dispersion, adding ammonia water and stirring uniformly, keeping at 30-35℃, adding an ethyl silicate ethanol solution at a uniform speed, keeping stirring for 3-5h, filtering the solid and drying to obtain the silicon dioxide coated zirconia; after being coated with silicon dioxide, the zirconia is coated with a dense protective layer, improving the stability.

[0016] The preparation of the modified silicon carbide includes the following steps: Step one: taking silicon carbide and amino silane (KH550), adding an ethanol aqueous solution and stirring uniformly, adjusting the pH to 4-5, heating to 50-60℃ and stirring for 3-6h, filtering the solid, washing, and drying to obtain amino silicon carbide; Step two: taking monomercapto-β-cyclodextrin and vinyl POSS, adding N,N-dimethylformamide and stirring uniformly, adding a photoinitiator, ultraviolet light irradiation for 2-4h, removing the solvent, washing, and drying to obtain modified dextrin; adding the modified dextrin to water, heating to 90-95℃ and stirring uniformly, adjusting the pH to 3-4, adding glutaraldehyde, keeping at 60-70℃ and stirring for 6-8h, removing the solvent, and washing to obtain aldehyde-modified dextrin; Step three: adding the aldehyde-modified dextrin to water, stirring uniformly at 60-70℃, adding amino silicon carbide, keeping stirring for 8-12h, filtering the solid, washing, and drying to obtain modified silicon carbide.

[0017] Silicon carbide has high hardness, which can improve the overall hardness and thermal shock resistance; at the same time, it has high thermal conductivity, which can quickly disperse the local thermal stress of zirconia, improving the stability. The addition of POSS can avoid the breakage of the structure bond of silicon dioxide, improving the overall density. Dextrin plays a role in lubrication and bonding, improving the processability of each powder in the blank raw material, thereby optimizing the overall quality.

[0018] More preferably, the silicon dioxide coated zirconia includes the following raw materials, in mass fraction: 1-2 parts of zirconium oxide, 0.5-0.6 parts of cetyltrimethylammonium bromide, 0.5-1 parts of ammonia water, and 0.3-0.6 parts of ethyl silicate; The amino silicon carbide includes the following raw materials, in mass fraction: 10-20 parts of silicon carbide and 1-2 parts of amino silane; The modified dextrin comprises the following raw materials in parts by mass: 1-2 parts of monothiol-beta-cyclodextrin, 0.3-0.6 parts of vinyl POSS, and 0.001-0.0015 parts of a photoinitiator; the aldehyde-modified dextrin comprises the following raw materials in parts by mass: 0.3-0.5 parts of modified dextrin, 30-50 parts of water, and 2-3 parts of glutaraldehyde. The modified silicon carbide comprises the following raw materials in parts by mass: 2-3 parts of aldehyde-modified dextrin, 100-150 parts of water, and 15-20 parts of aminosilicon carbide.

[0019] Compared with the prior art, the present application has the following advantages: (1) the zirconia composition is introduced, the micro-cracks generated by volume expansion during the phase transition of the zirconia composition are used to toughen the composition, the overall thermal shock resistance is improved, the amount of the zirconia composition is controlled, and the zirconia with a particle size of 1-2 um and a stabilizer are selected, so that the cracks are not superimposed into larger cracks, but the corrosion resistance and other properties are not reduced.

[0020] (2) In order to stabilize the zirconia and improve the overall performance, the yttrium-stabilized zirconia is selected as the stabilizer, the radius of Y ion is close to that of Zr ion, so that the phase transition of the zirconia can be inhibited by forming a solid solution to avoid instability caused by volume mutation; however, the amount of the yttrium-stabilized zirconia should not be too much, otherwise the toughening effect will be affected if the phase transition is completely inhibited.

[0021] (3) Since rare earth elements are relatively rare, the yttrium-stabilized zirconia is partially replaced by a combination of modified silicon carbide and silica-coated zirconia; the silica-coated zirconia forms a dense protective layer on the surface, which also plays a stabilizing role, and the introduction of silica improves the overall corrosion resistance; the silicon carbide has high thermal conductivity, which can quickly dissipate the local thermal stress of the zirconia and improve its stability; the silicon carbide is modified by dextrin and POSS, the addition of POSS can avoid the breakage of the structure bond of silica, improve the overall density, and thus improve the corrosion resistance; the dextrin plays a lubricating and bonding role to optimize the overall quality.

[0022] In summary, the tungsten alloy heater with thermal shock resistance and corrosion resistance is prepared by introducing the zirconia composition in a specific proportion. DETAILED DESCRIPTION

[0023] The technical solutions in the embodiments of the present application will be described below in a clear and complete manner. Obviously, the described embodiments are only some of the embodiments of the present application, but not all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0024] It should be noted that the purchase manufacturer of all raw materials involved in the present application has no special restriction, and exemplarily includes: tungsten alloy heating conductive paste (composition 99.9W-0.06Ni-0.04Fe); amino silane is KH550; photoinitiator is 2,2-dimethoxy-2-phenylacetophenone; monothiol-β-cyclodextrin (XK7772); vinyl POSS (XK3634); ammonia water (20wt%); alumina (3um); silicon carbide (1um); Unless otherwise specified, the following are all mass parts, mass ratio; Preparation of yttria-stabilized zirconia: take 95 parts of zirconia, 5 parts of yttria, 0.05 parts of alumina, and 0.01 parts of dispersant ammonium polymethacrylate, add water and stir uniformly to obtain a slurry with a solid content of 55wt%; ball mill for 1h, grinding body is zirconia ball with particle size of 6mm, ball mill speed is 160r / min; pour the milled slurry into a sand mill, add water to adjust the solid content to 35wt%, use zirconia beads with particle size of 0.8mm as grinding body, sand mill for 5h, sand mill speed is 2000r / min; spray drying, adjust the atomization frequency to 45Hz, the inlet air temperature is 240℃, the outlet air temperature is 90℃, 800℃ pre-burning for 2h, 1350℃ calcination for 4h, grinding and sieving, to obtain 4um yttria-stabilized zirconia.

[0025] Example 1: S1: take the zirconia composition with a mass ratio of 25:75, alumina, mix uniformly at a speed of 20000r / min, under the condition of temperature 60℃, pressure 120MPa, static pressure for 300s, cutting, to obtain an alumina blank with a width of 25mm, a length of 300mm, and a thickness of 1.15mm; S2: take an alumina blank, print tungsten alloy heating conductive paste as heating wire to obtain a lower alumina blank; when printing, reserve 20mm non-heating area for lead-out line, the heating wire width is 1.5mm, the design heating temperature is 1500℃, the working voltage is 660V, the working current is 1.31A, the resistance is 500Ω, 334Ω per meter, the printing heating wire length is 1500mm; S3: take another alumina blank as an upper alumina blank, stack it with the lower alumina blank prepared in S2, and press cast into a shape under the condition of 1630℃ and 1 ton pressure, to obtain a tungsten alloy heater with a thickness of 1.5mm; The zirconia composition is zirconia with a particle size of 2um and yttria-stabilized zirconia with a particle size of 4um, with a mass ratio of 15:85.

[0026] Embodiment 2: S1: Take the zirconium oxide composition, aluminum oxide with a mass ratio of 25:75, mix uniformly under the condition of 20000r / min, and under the condition of 60℃ and 120MPa, static pressure for 300s, cutting, to obtain an aluminum oxide blank with a width of 25mm, a length of 300mm, and a thickness of 1.15mm; S2: Take an aluminum oxide blank, print tungsten alloy heating conductive paste as a heating line to obtain a lower layer of aluminum oxide blank; when printing, reserve a non-heating area of 20mm for the lead-out line, the heating line has a width of 1.5mm, the design heating temperature is 1500℃, the working voltage is 660V, the working current is 1.31A, the resistance is 500Ω, 334Ω per meter, and the length of the printed heating line is 1500mm; S3: Take another aluminum oxide blank as an upper layer of aluminum oxide blank, and stack it with the lower layer of aluminum oxide blank prepared in S2, and press cast into a tungsten alloy heater with a thickness of 1.5mm under the condition of 1630℃ and 1 ton of pressure; The zirconium oxide composition is zirconium oxide with a particle size of 2um and a stabilizer with a mass ratio of 15:85; The stabilizer is yttrium oxide stabilized zirconium oxide with a particle size of 4um, silica coated zirconium oxide, and modified silicon carbide with a mass ratio of 1:12:0.6; Preparation of silica coated zirconium oxide: take 100 parts of 70wt% ethanol aqueous solution, 2 parts of zirconium oxide, and 0.5 parts of cetyltrimethylammonium bromide, ultrasonic dispersion for 0.5h, add 0.5 parts of ammonia water, stir uniformly, keep at 35℃, add the ethyl silicate ethanol solution (including 0.5 parts of ethyl silicate and 10 parts of ethanol) at a constant speed, 2h for dropwise addition, keep stirring for 4h, filter the solid, dry, and obtain silica coated zirconium oxide; Preparation of modified silicon carbide: take 10 parts of silicon carbide and 1 part of KH550, add into ethanol aqueous solution, adjust pH to 4.5, heat to 60℃, stir for 4h, filter the solid, wash, dry, and obtain aminated silicon carbide; Take 1 part of monothiol-β-cyclodextrin and 0.4 part of vinyl POSS, add into 15 parts of DMF, stir uniformly, add 0.001 part of 2,2-dimethoxy-2-phenylacetophenone, irradiate under 365nm ultraviolet lamp for 3h, remove the solvent, wash, dry, and obtain modified dextrin; add 0.4 part of modified dextrin into 50 parts of water, heat to 95℃, stir uniformly, adjust pH to 3, add 3 parts of glutaraldehyde, keep stirring at 70℃ for 7h, remove the solvent, wash, and obtain aldehyde modified dextrin; Add 3 parts of aldehyde modified dextrin into 150 parts of water, stir uniformly at 70℃, add 20 parts of aminated silicon carbide, keep stirring for 12h, filter the solid, wash, dry, and obtain modified silicon carbide.

[0027] Comparative Example 1 (increasing the amount of zirconia composition, the rest is the same as Example 2): S1: take the mass ratio of 35:65 of zirconia composition, alumina, mix uniformly under the condition of 20000r / min, under the condition of temperature 60℃, pressure 120MPa, static pressure 300s, cutting, get width 25mm, length 300mm, thickness 1.15mm alumina blank.

[0028] Comparative Example 2 (silicon carbide instead of modified silicon carbide, the rest is the same as Example 2): S1: take the mass ratio of 25:75 of zirconia composition, alumina, mix uniformly under the condition of 20000r / min, under the condition of temperature 60℃, pressure 120MPa, static pressure 300s, cutting, get width 25mm, length 300mm, thickness 1.15mm alumina blank; S2: take a piece of alumina blank, print tungsten alloy heating conductive paste as heating line, get lower alumina blank; when printing, reserve 20mm non-heating area for lead-out line, the width of heating line is 1.5mm, the design heating temperature is 1500℃, the working voltage is 660V, the working current is 1.31A, the resistance is 500Ω, 334Ω per meter, the length of printed heating line is 1500mm; S3: take another piece of alumina blank as upper alumina blank, stack with the lower alumina blank prepared in S2, pressure casting at 1630℃ under 1 ton pressure, get tungsten alloy heater with thickness 1.5mm; The zirconia composition is 15:85 of particle size 2um zirconia and stabilizer by mass ratio; The stabilizer is 1:12:0.6 of particle size 4um yttria stabilized zirconia, silica coated zirconia and silicon carbide by mass ratio; Preparation of silica coated zirconia: take 100 parts of 70wt% ethanol aqueous solution, 2 parts of zirconia, 0.5 parts of cetyltrimethylammonium bromide, ultrasonic dispersion for 0.5h, add 0.5 parts of ammonia water, stir uniformly, keep 35℃, add ethyl silicate ethanol solution (including 0.5 parts of ethyl silicate and 10 parts of ethanol) at a constant speed, 2h for dropwise addition, keep stirring for 4h, filter the solid, dry, get silica coated zirconia.

[0029] Comparative Example 3 (silicon carbide mixture instead of silicon carbide, the rest is the same as Example 2): S1: take the mass ratio of 25:75 of zirconia composition, alumina, mix uniformly under the condition of 20000r / min, under the condition of temperature 60℃, pressure 120MPa, static pressure 300s, cutting, get width 25mm, length 300mm, thickness 1.15mm alumina blank; S2: Take a piece of alumina blank, print tungsten alloy heating and conductive paste, use this as the heating wire to obtain the lower layer of alumina blank; during printing, reserve a 20mm non-heating area for the lead wire, the width of the heating wire is 1.5mm, the designed heating temperature is 1500℃, the working voltage is 660V, the working current is 1.31A, the resistance is 500Ω, 334Ω per meter, and the length of the printed heating line is 1500mm; S3: Take another alumina billet as the upper alumina billet, stack it with the lower alumina billet prepared in S2, and die-cast it at 1630℃ and 1 ton of pressure to obtain a tungsten alloy heater with a thickness of 1.5mm. The zirconium oxide composition consists of zirconium oxide with a particle size of 2 μm in a mass ratio of 15:85, and a stabilizer. The stabilizer is a mixture of yttrium-stabilized zirconium oxide, silica-coated zirconium oxide, and silicon carbide with a particle size of 4 μm in a mass ratio of 1:12:0.6. Preparation of silica-coated zirconium oxide: Take 100 parts of 70wt% ethanol aqueous solution, 2 parts of zirconium oxide, and 0.5 parts of hexadecyltrimethylammonium bromide, and ultrasonically disperse for 0.5 h. Add 0.5 parts of ammonia water, stir evenly, and keep at 35℃. Add ethanol solution of tetraethyl orthosilicate (including 0.5 parts of tetraethyl orthosilicate and 10 parts of ethanol) dropwise at a uniform rate. The addition is completed in 2 h. Keep warm and stir for 4 h. Filter to take solid, dry, and obtain silica-coated zirconium oxide. Preparation of silicon carbide mixture: Take 1 part of monothiol-β-cyclodextrin and 0.4 parts of vinyl POSS, mix them to obtain dextrin-POSS mixture; Three parts of dextrin-POSS mixture were mixed with 20 parts of silicon carbide to obtain a silicon carbide mixture.

[0030] Comparative Example 4 (with increased amount of modified silicon carbide, otherwise the same as Example 2): S1: Take a zirconium oxide composition and alumina in a mass ratio of 25:75, mix them evenly at a speed of 20000 r / min, and then statically press them for 300s at a temperature of 60℃ and a pressure of 120MPa to obtain an alumina billet with a width of 25mm, a length of 300mm and a thickness of 1.15mm. S2: Take a piece of alumina blank, print tungsten alloy heating and conductive paste, use this as the heating wire to obtain the lower layer of alumina blank; during printing, reserve a 20mm non-heating area for the lead wire, the width of the heating wire is 1.5mm, the designed heating temperature is 1500℃, the working voltage is 660V, the working current is 1.31A, the resistance is 500Ω, 334Ω per meter, and the length of the printed heating line is 1500mm; S3: Take another alumina billet as the upper alumina billet, stack it with the lower alumina billet prepared in S2, and die-cast it at 1630℃ and 1 ton of pressure to obtain a tungsten alloy heater with a thickness of 1.5mm. The zirconium oxide composition is 15:85 of zirconium oxide with a particle size of 2um, a stabilizer by mass ratio; The stabilizer is 1:12:2 of yttrium oxide stabilized zirconium oxide with a particle size of 4um, silica coated zirconium oxide, and modified silicon carbide by mass ratio; Preparation of silica coated zirconium oxide: take 100 parts of 70wt% ethanol aqueous solution, 2 parts of zirconium oxide, 0.5 parts of cetyltrimethylammonium bromide, ultrasonic dispersion for 0.5h, add 0.5 parts of ammonia water, stir uniformly, keep 35℃, add the ethanol solution of tetraethyl orthosilicate (including 0.5 parts of tetraethyl orthosilicate and 10 parts of ethanol) at a constant speed, 2h for dropping, keep stirring for 4h, filter the solid, dry, and get silica coated zirconium oxide; Preparation of modified silicon carbide: take 10 parts of silicon carbide, 1 part of KH550, add into ethanol aqueous solution, adjust pH to 4.5, heat to 60℃, stir for 4h, filter the solid, wash, dry, and get aminated silicon carbide; Take 1 part of monothiol-β-cyclodextrin, 0.4 part of vinyl POSS, add into 15 parts of DMF and stir uniformly, add 0.001 part of 2,2-dimethoxy-2-phenylacetophenone, irradiate under 365nm ultraviolet lamp for 3h, remove the solvent, wash, dry, and get modified dextrin; add 0.4 part of modified dextrin into 50 parts of water, heat to 95℃ and stir uniformly, adjust pH to 3, add 3 parts of glutaraldehyde, keep 70℃ and stir for 7h, remove the solvent, wash, and get aldehyde modified dextrin; Add 3 parts of aldehyde modified dextrin into 150 parts of water, stir uniformly at 70℃, add 20 parts of aminated silicon carbide, keep stirring for 12h, filter the solid, wash, dry, and get modified silicon carbide.

[0031] Performance test 1: take the tungsten alloy heater prepared in examples 1~2 and comparative examples 1~4; (1) weigh, boil in 30wt% sulfuric acid for 48h, wash and dry, weigh again, calculate the corrosion amount, unit: mg / cm 2 ; (2) perform thermal shock test: heat to 1000℃, keep for 20min, take out and put into 20℃ water for cooling; repeat the above thermal shock test until peeling or cracking occurs, record the number of thermal shock resistance; see table 1 for details; Table 1:

[0032] The micro-cracks caused by the increased amount of zirconium oxide composition in Comparative Example 1 are superimposed into larger cracks, resulting in a significant decrease in performance; in Comparative Example 2, silicon carbide is used instead of modified silicon carbide, and in Comparative Example 3, the silicon carbide is not modified, but only mixed with dextrin and POSS and then added, both of which result in a decrease in performance, thus indicating the importance of the modification of silicon carbide; in Comparative Example 4, the amount of modified silicon carbide is increased, and the inhibition of zirconium oxide is too strong, resulting in a decrease in toughening effect and a significant decrease in thermal shock resistance. In summary, the tungsten alloy heater prepared by the present scheme has excellent corrosion resistance and thermal shock resistance.

[0033] Finally, it should be noted that the above description is only a preferred embodiment of the present application and is not intended to limit the present application. Although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art can modify the technical solutions described in the foregoing embodiments or make equivalent replacements to some technical features. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application shall be included in the protection scope of the present application.

Claims

1. A manufacturing process for a high-efficiency tungsten alloy heater, characterized in that: Includes the following steps: S1: Mix the zirconium oxide composition and alumina in a mass ratio of (20~26):(74~80), press them into shape, and obtain alumina billet; S2: Take an alumina blank, print tungsten alloy heating and conductive paste to form heating wires, then cover it with the alumina blank and die-cast it to obtain a tungsten alloy heater.

2. The preparation process of the high-efficiency tungsten alloy heater according to claim 1, characterized in that: The alumina blank has a width of 20-25mm, a length of 300mm, and a thickness of 1.15mm; the heating wire is 1.5mm wide, and a 20mm non-heating area is reserved for the lead-out wire during printing.

3. The preparation process of the high-efficiency tungsten alloy heater according to claim 1, characterized in that: In S1, the compression molding process is as follows: static pressure is applied for 300-350 seconds at 60-65℃ and 100-120MPa. In S2, the die-casting process is: die-casting at 1600~1650℃ and 1 ton.

4. The preparation process of the high-efficiency tungsten alloy heater according to claim 1, characterized in that: The zirconium oxide composition is zirconium oxide and stabilizer in a mass ratio of (10~15):(85~90).

5. The preparation process of the high-efficiency tungsten alloy heater according to claim 4, characterized in that: The stabilizer includes yttrium oxide-stabilized zirconium oxide, the particle size of which is 2-5 μm; and the particle size of which is 1-2 μm.

6. The preparation process of the high-efficiency tungsten alloy heater according to claim 5, characterized in that: The stabilizer is yttrium-stabilized zirconium oxide, silica-coated zirconium oxide, or modified silicon carbide in a mass ratio of (1~2):(10~15):(0.5~0.8).

7. The preparation process of the high-efficiency tungsten alloy heater according to claim 6, characterized in that: The preparation of the silica-coated zirconium oxide includes the following steps: Take an aqueous ethanol solution, zirconium oxide, and hexadecyltrimethylammonium bromide, disperse them by ultrasonication, add ammonia water and stir evenly, keep at 30~35℃, add an ethanol solution of tetraethyl orthosilicate dropwise at a uniform rate, keep warm and stir for 3~5h, filter to collect the solid, dry it, and obtain silica-coated zirconium oxide.

8. The preparation process of the high-efficiency tungsten alloy heater according to claim 6, characterized in that: The preparation of the modified silicon carbide includes the following steps: Step 1: Take silicon carbide and aminosilane, add them to an ethanol aqueous solution and stir evenly, adjust the pH to 4~5, heat to 50~60℃ and stir for 3~6 hours, filter to take the solid, wash and dry to obtain amino-modified silicon carbide. Step 2: Take monothiol-β-cyclodextrin and vinyl POSS, add them to N,N-dimethylformamide and stir well. Add photoinitiator, irradiate with ultraviolet light for 2-4 hours, remove solvent, wash and dry to obtain modified dextrin. Add the modified dextrin to water, heat to 90-95℃ and stir until homogeneous, adjust the pH to 3-4, add glutaraldehyde, maintain 60-70℃ and stir for 6-8 hours, remove the solvent and wash to obtain aldehyde-modified dextrin. Step 3: Add the aldehyde-modified dextrin to water, stir evenly at 60~70℃, add the aminated silicon carbide, keep warm and stir for 8~12 hours, filter to obtain the solid, wash and dry to obtain modified silicon carbide.

9. The preparation process of the high-efficiency tungsten alloy heater according to claim 7, characterized in that: The silica-coated zirconium oxide comprises the following raw materials, by mass parts: 1-2 parts zirconium oxide, 0.5-0.6 parts hexadecyltrimethylammonium bromide, 0.5-1 parts ammonia water, and 0.3-0.6 parts tetraethyl orthosilicate.

10. The preparation process of the high-efficiency tungsten alloy heater according to claim 8, characterized in that: The aminated silicon carbide comprises the following raw materials, by mass parts: 10-20 parts silicon carbide, 1-2 parts aminosilane; The modified dextrin comprises the following raw materials, by weight: 1-2 parts monothiol-β-cyclodextrin, 0.3-0.6 parts vinyl POSS, and 0.001-0.0015 parts photoinitiator; the aldehyde-modified dextrin comprises the following raw materials, by weight: 0.3-0.5 parts modified dextrin, 30-50 parts water, and 2-3 parts glutaraldehyde; The modified silicon carbide comprises the following raw materials, by mass: 2-3 parts aldehyde-modified dextrin, 100-150 parts water, and 15-20 parts amino-modified silicon carbide.

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