CN110563464A - High-temperature-resistant and oxidation-resistant graphite mold and preparation method thereof - Google Patents
High-temperature-resistant and oxidation-resistant graphite mold and preparation method thereof Download PDFInfo
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- C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
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Abstract
the invention discloses a high-temperature-resistant and oxidation-resistant graphite mold and a preparation method thereof, wherein the mold material comprises, by weight, 15-25% of asphalt, 3-5% of silicon nitride, 0.3-0.8% of titanium nitride, 0.1-0.5% of yttrium and 0.1-0.5% of erbium; the balance being graphite. The preparation method comprises the steps of adding graphite and asphalt into a kneading machine, kneading, then putting into a die, compacting, vacuumizing, then sending into an isostatic press for static pressure forming, and demoulding to obtain a raw blank; roasting the green blank under the protection of inert gas; placing the roasted graphite block into an antioxidant impregnant for pressure impregnation treatment, and roasting the impregnated graphite for the second time; and coating the surface of the roasted graphite module with silicon carbide and zirconium oxide mixed slurry, airing, and putting into a graphite furnace for high-temperature graphitization treatment to prepare the graphite mold for hot press molding. The graphite mold prepared by the invention has good oxidation resistance, compressive strength and conductivity under high temperature.
Description
Technical Field
the invention belongs to the technical field of molds, and particularly relates to a high-temperature-resistant and oxidation-resistant graphite mold and a preparation method thereof.
background
The mould is basic technological equipment widely used in industrial production, and the mould industry is the basic industry of national economy. In modern industrial production, product parts are widely processed by stamping, hot press forming, forging forming, die-casting forming, extrusion forming, plastic injection or other forming processing methods, and are matched with forming dies to form blanks into parts meeting product requirements. The shape of the mold determines the shape of the products, and the processing quality and precision of the mold determine the quality of the products. In recent years, the mold industry has been rapidly developed, and graphite materials, new processes and increasing mold factories have continuously impacted the mold market.
Graphite has excellent electric conductivity, heat conductivity and self-lubricating property and higher mechanical strength, so that the graphite material is widely applied to the fields of machinery, electronics, semiconductors, metallurgy, chemical industry and the like and becomes an important special engineering material in modern industry. However, the graphite material has a weak point that it is poor in high-temperature oxidation resistance and is easily oxidized at high temperature, and generally, the oxidation corrosion rate of graphite is rapidly increased from 450 ℃ to more than 750 ℃. The oxidation has a great influence on the mechanical properties of the graphite mold material, the hardness and the breaking strength of the graphite mold are reduced along with the increase of oxidation weight loss, the surface pores and the surface roughness of the mold are increased, the appearance and the size precision are reduced, and the service life of the graphite mold is seriously influenced. Therefore, how to improve the oxidation resistance of the graphite mold at high temperature is the focus of research at present.
The above background disclosure is only for the purpose of assisting understanding of the inventive concept and technical solutions of the present invention, and does not necessarily belong to the prior art of the present patent application, and should not be used for evaluating the novelty and inventive step of the present application in the case that there is no clear evidence that the above content is disclosed at the filing date of the present patent application.
Disclosure of Invention
The invention provides a high-temperature-resistant and oxidation-resistant graphite mold and a preparation method thereof, aiming at the problems of the existing graphite mold. The graphite mold prepared by the invention has good oxidation resistance, compressive strength and conductivity under high temperature.
in order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the high-temperature-resistant and oxidation-resistant graphite mold comprises, by weight, 15-25% of asphalt, 3-5% of silicon nitride, 0.3-0.8% of titanium nitride, 0.1-0.5% of yttrium and 0.1-0.5% of erbium; the balance being graphite.
Preferably, the graphite is flake graphite.
The invention also provides a preparation method of the high-temperature-resistant and antioxidant graphite mold, which comprises the following steps:
(1, adding graphite and asphalt into a kneading machine, kneading for 30-60min, and cooling to obtain a mixed material;
(2) Putting the mixed material into a mold, compacting and vacuumizing, then sending into an isostatic press for static pressure forming, and demolding to obtain a raw blank;
(3) Roasting the green blank for 1-2h under the protection of inert gas, wherein the roasting temperature is 900-1100 ℃, and obtaining graphite blocks;
(4) Putting the roasted graphite block into an antioxidant impregnant for pressure impregnation treatment for 3-6h, wherein the antioxidant impregnant comprises the following raw materials: aluminum dihydrogen phosphate, sodium pyrophosphate, sodium tungstate, barium oxide, strontium carbonate, sodium fluoride, tributyl borate, triethanolamine and water.
(5) Heating the graphite block after the dipping treatment to 400-500 ℃, keeping the temperature, roasting for 0.5-1.5h, then heating to 850-950 ℃, keeping the temperature for 0.5-1.0h, and cooling to room temperature;
(6) And (3) coating the surface of the graphite module roasted in the step (5) with mixed slurry containing silicon nitride, titanium nitride, yttrium and erbium, airing, putting into a graphite furnace, heating to 1500-1600 ℃, preserving heat for 1-2h, heating to 2200-2400 ℃, preserving heat for 3-5h, and thus obtaining the high-temperature-resistant and antioxidant graphite mold.
Preferably, the antioxidant impregnant comprises the following components in percentage by weight: 10-20% of aluminum dihydrogen phosphate, 3-5% of sodium pyrophosphate, 0.5-1.5% of sodium tungstate, 0.1-0.5% of barium oxide, 0.1-0.3% of strontium carbonate, 0.3-0.8% of sodium fluoride, 0.5-1.5% of tributyl borate, 1-3% of triethanolamine and the balance of water.
Preferably, the mixed slurry is prepared by putting silicon nitride, titanium nitride, yttrium and erbium in nitrile rubber, rosin resin and polymethylphenylsiloxane.
preferably, the weight percentage of the nitrile rubber, the rosin resin and the polymethylphenylsiloxane in the slurry is 60-80%, wherein the mass ratio of the nitrile rubber, the rosin resin and the polymethylphenylsiloxane is 1:0.5-1.5: 2-4.
preferably, the kneading is carried out at a rotation speed of 100-150r/min and a temperature of 150-180 ℃.
Preferably, the static pressure forming is that the pressure is increased to 80-120MPa at the pressure increasing rate of 5-8MPa/min and stabilized for 20-30min, and then the pressure is released to 40-60MPa at the pressure releasing rate of 15-20MPa/min and stabilized for 10-15 min; finally, the pressure is released to room pressure at the pressure release rate of 10-15 MPa/min.
Preferably, the pressure impregnation treatment is carried out under the pressure of 0.3-0.5MPa and the temperature of 150-180 ℃.
Preferably, the heating rate of the roasting in the step (3) and the step (5) is 5-10 ℃/min.
compared with the prior art, the invention has the advantages and beneficial effects that:
1. the graphite mold is prepared by taking graphite, asphalt, titanium nitride, yttrium and erbium as raw materials and carrying out processes of mixing kneading molding, roasting, pressurizing impregnation and the like, and due to the coordination of the components and the optimization of the processes, the prepared graphite mold has excellent compression strength performance and good oxidation resistance at high temperature, the service life of the mold is prolonged, and the strength is improved.
2. According to the invention, the surface of the graphite block is coated with the mixed slurry of silicon nitride, titanium nitride, yttrium and erbium, and then high-temperature graphitization treatment is carried out, so that a compact antioxidation layer can be formed on the surface of the graphite, the oxidation resistance of the mold can be obviously improved at high temperature, and the strength of the mold can be improved
3. the antioxidant impregnant provided by the invention consists of aluminum dihydrogen phosphate, sodium pyrophosphate, sodium tungstate, barium oxide, strontium carbonate, sodium fluoride, tributyl borate, triethanolamine and water, and can obviously improve the oxidation resistance of graphite without reducing the electrical property and the mechanical property of the graphite due to the coordination of the components.
Detailed Description
the present invention will be described in further detail with reference to specific embodiments. It should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
example 1
A high temperature resistant oxidation resistant graphite mould comprises 20% of asphalt, 3% of silicon nitride, 0.5% of titanium nitride, 0.3% of yttrium and 0.2% of erbium by weight percentage; the balance being graphite.
The preparation method comprises the following steps:
(1, adding graphite and asphalt into a kneading machine, kneading for 45min at the rotating speed of 120r/min and the temperature of 160 ℃, and cooling to obtain a mixed material;
(2) putting the mixed material into a mold, compacting and vacuumizing, then sending into an isostatic press for static pressure forming, and demolding to obtain a raw blank; the static pressure forming is to increase the pressure to 100MPa at the pressure increasing rate of 5MPa/min and stabilize the pressure for 20min, and then to release the pressure to 50MPa at the pressure releasing rate of 20MPa/min and stabilize the pressure for 10 min; finally, the pressure is released to room pressure at the pressure release rate of 15 MPa/min.
(3) Roasting the green blank for 1.5h under the protection of inert gas, wherein the roasting temperature is 900-1100 ℃, and obtaining graphite blocks;
(4) Putting the roasted graphite block into an antioxidant impregnant for pressure impregnation treatment for 3-6h, wherein the antioxidant impregnant comprises the following raw materials: 18% of aluminum dihydrogen phosphate, 4% of sodium pyrophosphate, 1.2% of sodium tungstate, 0.3% of barium oxide, 0.2% of strontium carbonate, 0.5% of sodium fluoride, 1.2% of tributyl borate, 2% of triethanolamine and the balance of water.
(5) heating the graphite block after the dipping treatment to 450 ℃, preserving heat, roasting for 1h, then heating to 900 ℃, preserving heat for 1.0h, and cooling to room temperature;
(6) and (3) coating the surface of the graphite module roasted in the step (5) with mixed slurry containing silicon nitride, titanium nitride, yttrium and erbium, airing, putting into a graphite furnace, heating to 1550 ℃, keeping the temperature for 1.5h, heating to 2300 ℃, and keeping the temperature for 4h to obtain the high-temperature-resistant and antioxidant graphite mold. The mixed slurry is prepared by putting silicon nitride, titanium nitride, yttrium and erbium in nitrile rubber, rosin resin and polymethylphenylsiloxane; the weight percentage of the nitrile rubber, the rosin resin and the polymethylphenylsiloxane in the slurry is 75%, wherein the mass ratio of the nitrile rubber to the rosin resin to the polymethylphenylsiloxane is 1:0.5: 3.
Example 2
A high temperature resistant oxidation resistant graphite mould comprises 15% of asphalt, 5% of silicon nitride, 0.6% of titanium nitride, 0.2% of yttrium and 0.5% of erbium by weight percentage; the balance being graphite.
The preparation method comprises the following steps:
(1) adding graphite and asphalt into a kneading machine, kneading for 30min at the rotating speed of 150r/min and the temperature of 180 ℃, and cooling to obtain a mixed material;
(2) Putting the mixed material into a mold, compacting and vacuumizing, then sending into an isostatic press for static pressure forming, and demolding to obtain a raw blank; the static pressure forming is to increase the pressure increasing rate to 120MPa at the pressure increasing rate of 8MPa/min and stabilize the pressure for 30min, then to release the pressure to 60MPa at the pressure releasing rate of 15MPa/min and stabilize the pressure for 15 min; finally, the pressure is released to room pressure at the pressure release rate of 10 MPa/min.
(3) Roasting the green blank for 1h under the protection of inert gas, wherein the roasting temperature is 1000 ℃, and obtaining graphite blocks;
(4) Putting the roasted graphite block into an antioxidant impregnant for pressure impregnation treatment for 5 hours, wherein the antioxidant impregnant comprises the following raw materials: 20% of aluminum dihydrogen phosphate, 3% of sodium pyrophosphate, 0.8% of sodium tungstate, 0.2% of barium oxide, 0.3% of strontium carbonate, 0.8% of sodium fluoride, 1.5% of tributyl borate, 3% of triethanolamine and the balance of water.
(5) heating the graphite block after the dipping treatment to 450 ℃, preserving heat, roasting for 1h, then heating to 900 ℃, preserving heat for 1.0h, and cooling to room temperature;
(6) And (3) coating the surface of the graphite module roasted in the step (5) with mixed slurry containing silicon nitride, titanium nitride, yttrium and erbium, airing, putting into a graphite furnace, heating to 1600 ℃, preserving heat for 1h, heating to 2400 ℃, preserving heat for 3.5h, and preparing the high-temperature-resistant and antioxidant graphite mold. The mixed slurry is prepared by putting silicon nitride, titanium nitride, yttrium and erbium in nitrile rubber, rosin resin and polymethylphenylsiloxane; the weight percentage of the nitrile rubber, the rosin resin and the polymethylphenylsiloxane in the slurry is 70%, wherein the mass ratio of the nitrile rubber to the rosin resin to the polymethylphenylsiloxane is 1:1: 2.
Example 3
A high temperature resistant oxidation resistant graphite mould comprises 20% of asphalt, 3.5% of silicon nitride, 0.6% of titanium nitride, 0.4% of yttrium and 0.3% of erbium by weight percentage; the balance being graphite.
The preparation method comprises the following steps:
(1, adding graphite and asphalt into a kneading machine, kneading for 60min at the rotating speed of 120r/min and the temperature of 170 ℃, and cooling to obtain a mixed material;
(2) Putting the mixed material into a mold, compacting and vacuumizing, then sending into an isostatic press for static pressure forming, and demolding to obtain a raw blank; the static pressure forming is to increase the pressure increasing rate to 120MPa at the pressure increasing rate of 8MPa/min and stabilize the pressure for 30min, then to release the pressure to 60MPa at the pressure releasing rate of 15MPa/min and stabilize the pressure for 15 min; finally, the pressure is released to room pressure at the pressure release rate of 10 MPa/min.
(3) Roasting the green blank for 0.5h under the protection of inert gas, wherein the roasting temperature is 1100 ℃, and obtaining graphite blocks;
(4) putting the roasted graphite block into an antioxidant impregnant for pressure impregnation treatment for 4 hours, wherein the antioxidant impregnant comprises the following raw materials: 13% of aluminum dihydrogen phosphate, 4% of sodium pyrophosphate, 1.2% of sodium tungstate, 0.3% of barium oxide, 0.2% of strontium carbonate, 0.6% of sodium fluoride, 1.5% of tributyl borate, 1.5% of triethanolamine and the balance of water.
(5) Heating the graphite block after the dipping treatment to 400 ℃, keeping the temperature, roasting for 1.5h, then heating to 1050 ℃, keeping the temperature for 0.5h, and cooling to room temperature;
(6) And (3) coating the surface of the graphite module roasted in the step (5) with mixed slurry containing silicon nitride, titanium nitride, yttrium and erbium, airing, putting into a graphite furnace, heating to 1500 ℃, preserving heat for 2 hours, heating to 2350 ℃, preserving heat for 5 hours, and preparing the high-temperature-resistant and antioxidant graphite mold. The mixed slurry is prepared by putting silicon nitride, titanium nitride, yttrium and erbium in nitrile rubber, rosin resin and polymethylphenylsiloxane; the weight percentage of the nitrile rubber, the rosin resin and the polymethylphenylsiloxane in the slurry is 65%, wherein the mass ratio of the nitrile rubber to the rosin resin to the polymethylphenylsiloxane is 1:1.5: 2.5.
Example 4
A high temperature resistant oxidation resistant graphite mould comprises 18 percent of asphalt, 4.5 percent of silicon nitride, 0.4 percent of titanium nitride, 0.3 percent of yttrium and 0.2 percent of erbium by weight percentage; the balance being graphite.
the preparation method comprises the following steps:
(1, adding graphite and asphalt into a kneading machine, kneading for 60min at the rotating speed of 150r/min and the temperature of 170 ℃, and cooling to obtain a mixed material;
(2) Putting the mixed material into a mold, compacting and vacuumizing, then sending into an isostatic press for static pressure forming, and demolding to obtain a raw blank; the static pressure forming is to increase the pressure increasing rate to 80MPa at 6MPa/min and stabilize the pressure for 20min, then to release the pressure to 40MPa at 20MPa/min and stabilize the pressure for 10 min; finally, the pressure is released to room pressure at the pressure release rate of 15 MPa/min.
(3) Roasting the green blank for 1h under the protection of inert gas, wherein the roasting temperature is 1050 ℃, and obtaining graphite blocks;
(4) putting the roasted graphite block into an antioxidant impregnant for pressure impregnation treatment for 4 hours, wherein the antioxidant impregnant comprises the following raw materials: 13% of aluminum dihydrogen phosphate, 4% of sodium pyrophosphate, 1.2% of sodium tungstate, 0.3% of barium oxide, 0.2% of strontium carbonate, 0.6% of sodium fluoride, 1.5% of tributyl borate, 1.5% of triethanolamine and the balance of water.
(5) heating the graphite block after the dipping treatment to 400 ℃, keeping the temperature, roasting for 1.5h, then heating to 1050 ℃, keeping the temperature for 0.5h, and cooling to room temperature;
(6) and (3) coating the surface of the graphite module roasted in the step (5) with mixed slurry containing silicon nitride, titanium nitride, yttrium and erbium, airing, putting into a graphite furnace, heating to 1500 ℃, preserving heat for 2 hours, heating to 2350 ℃, preserving heat for 5 hours, and preparing the high-temperature-resistant and antioxidant graphite mold. The mixed slurry is prepared by putting silicon nitride, titanium nitride, yttrium and erbium in nitrile rubber, rosin resin and polymethylphenylsiloxane; the weight percentage of the nitrile rubber, the rosin resin and the polymethylphenylsiloxane in the slurry is 80%, wherein the mass ratio of the nitrile rubber to the rosin resin to the polymethylphenylsiloxane is 1:1.5: 2.5.
testing the compressive strength of the prepared graphite mold according to the GB/T1431-2009 standard; the resistivity is tested according to GB/T1410-2006; shore hardness was measured according to GB/T4341-2001 standard. The oxidation weight loss rate of graphite and the oxidation rate at 1000 ℃ were measured according to a conventional method, and the test results are shown in table 1.
Table 1: performance test results of the graphite mold prepared by the invention
From the test results, the graphite mold prepared by the invention has excellent compressive strength performance and good oxidation resistance at high temperature, the service life of the mold is prolonged, and the strength is improved.
the foregoing is a more detailed description of the invention in connection with specific/preferred embodiments and is not intended to limit the practice of the invention to those descriptions. It will be apparent to those skilled in the art that various substitutions and modifications can be made to the described embodiments without departing from the spirit of the invention, and such substitutions and modifications are to be considered as within the scope of the invention.
Claims (10)
1. a high temperature resistant anti-oxidation graphite mould which is characterized in that: the mould material comprises 15-25% of asphalt, 3-5% of silicon nitride, 0.3-0.8% of titanium nitride, 0.1-0.5% of yttrium and 0.1-0.5% of erbium by weight percentage; the balance being graphite.
2. The high temperature resistant and oxidation resistant graphite mold of claim 1, wherein: the graphite is flake graphite.
3. The method for preparing the high-temperature-resistant and oxidation-resistant graphite mold as claimed in claim 1, wherein the method comprises the following steps: the method comprises the following steps:
(1, adding graphite and asphalt into a kneading machine, kneading for 30-60min, and cooling to obtain a mixed material;
(2) Putting the mixed material into a mold, compacting and vacuumizing, then sending into an isostatic press for static pressure forming, and demolding to obtain a raw blank;
(3) Roasting the green blank for 1-2h under the protection of inert gas, wherein the roasting temperature is 900-1100 ℃, and obtaining graphite blocks;
(4) Putting the roasted graphite block into an antioxidant impregnant for pressure impregnation treatment for 3-6h, wherein the antioxidant impregnant comprises the following raw materials: aluminum dihydrogen phosphate, sodium pyrophosphate, sodium tungstate, barium oxide, strontium carbonate, sodium fluoride, tributyl borate, triethanolamine and water;
(5) heating the graphite block after the dipping treatment to 400-500 ℃, keeping the temperature, roasting for 0.5-1.5h, then heating to 850-950 ℃, keeping the temperature for 0.5-1.0h, and cooling to room temperature;
(6) And (3) coating the surface of the graphite module roasted in the step (5) with mixed slurry containing silicon nitride, titanium nitride, yttrium and erbium, airing, putting into a graphite furnace, heating to 1500-1600 ℃, preserving heat for 1-2h, heating to 2200-2400 ℃, preserving heat for 3-5h, and thus obtaining the high-temperature-resistant and antioxidant graphite mold.
4. The method for preparing the high-temperature-resistant and antioxidant graphite mold as claimed in claim 3, wherein the method comprises the following steps: the antioxidant impregnant comprises the following components in percentage by weight: 10-20% of aluminum dihydrogen phosphate, 3-5% of sodium pyrophosphate, 0.5-1.5% of sodium tungstate, 0.1-0.5% of barium oxide, 0.1-0.3% of strontium carbonate, 0.3-0.8% of sodium fluoride, 0.5-1.5% of tributyl borate, 1-3% of triethanolamine and the balance of water.
5. The method for preparing the high-temperature-resistant and antioxidant graphite mold as claimed in claim 3, wherein the method comprises the following steps: the mixed slurry is prepared by putting silicon nitride, titanium nitride, yttrium and erbium in nitrile rubber, rosin resin and polymethylphenylsiloxane.
6. the method for preparing the high-temperature-resistant and antioxidant graphite mold as claimed in claim 5, wherein the method comprises the following steps: the weight percentage of the nitrile rubber, the rosin resin and the polymethylphenyl siloxane in the slurry is 60-80%, wherein the mass ratio of the nitrile rubber, the rosin resin and the polymethylphenyl siloxane is 1:0.5-1.5:2-: 4.
7. the method for preparing the high-temperature-resistant and antioxidant graphite mold as claimed in claim 3, wherein the method comprises the following steps: the kneading is carried out at a rotation speed of 100-150r/min and a temperature of 150-180 ℃.
8. The method for preparing the high-temperature-resistant and antioxidant graphite mold as claimed in claim 3, wherein the method comprises the following steps: the static pressure forming is to increase the pressure increasing rate to 80-120MPa at the pressure increasing rate of 5-8MPa/min and stabilize the pressure for 20-30min, and then to release the pressure to 40-60MPa at the pressure releasing rate of 15-20MPa/min and stabilize the pressure for 10-15 min; finally, the pressure is released to room pressure at the pressure release rate of 10-15 MPa/min.
9. The method for preparing the high-temperature-resistant and oxidation-resistant graphite mold according to claim 3, wherein: the pressure impregnation treatment is carried out under the pressure of 0.3-0.5MPa and the temperature of 150-180 ℃.
10. The method for preparing the high-temperature-resistant and oxidation-resistant graphite mold according to claim 3, wherein: and (4) the temperature rising rate of the roasting in the step (3) and the step (5) is 5-10 ℃/min.
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| CN201910936291.8A CN110563464A (en) | 2019-09-29 | 2019-09-29 | High-temperature-resistant and oxidation-resistant graphite mold and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114773065A (en) * | 2022-04-13 | 2022-07-22 | 廊坊中英石棉化工有限公司 | High and low temperature resistant graphite pad and preparation method thereof |
| CN115626827A (en) * | 2022-12-19 | 2023-01-20 | 山东红点新材料有限公司 | Method for rapidly preparing carbon product by microwave roasting |
| CN115677369A (en) * | 2021-11-30 | 2023-02-03 | 江苏金亚隆科技有限公司 | Graphite shell for thermal power plant and preparation process thereof |
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Application publication date: 20191213 |