CN104045376A - Surface treatment method for improving high temperature oxidation resistance of silicon steel graphite roller sleeve - Google Patents
Surface treatment method for improving high temperature oxidation resistance of silicon steel graphite roller sleeve Download PDFInfo
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- CN104045376A CN104045376A CN201310082485.9A CN201310082485A CN104045376A CN 104045376 A CN104045376 A CN 104045376A CN 201310082485 A CN201310082485 A CN 201310082485A CN 104045376 A CN104045376 A CN 104045376A
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- roller shell
- high temperature
- silicon steel
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Abstract
The invention discloses a surface treatment method for improving the high temperature oxidation resistance of a silicon steel graphite roller sleeve. The method comprises the steps of: 1. Roller sleeve substrate surface treatment; 2. immersion treatment; 3. medium temperature curing treatment; and 4. non-oxidation pyrolysis ceramic treatment. Specifically, the roller sleeve substrate is a graphite substrate; the roller sleeve surface treatment enables better combination of an anti-oxidation coating layer and the roller sleeve substrate; the immersion solution adopted by the immersion treatment is liquid polycarbosilane; the curing temperature of the medium temperature curing treatment is 150-200DEG C; and the temperature of the non-oxidation pyrolysis ceramic treatment is 1000-1200DEG C. By adopting the technical scheme involved in the invention, the physical properties of the graphite roller sleeve can be changed, the volume density can be increased, and the apparent porosity can be reduced, so that the antioxidation ability of the graphite roller sleeve can be improved.
Description
Technical field
The present invention relates to a kind of surface treatment method, more particularly, relate to a kind of surface treatment method that improves silicon steel graphite roller shell high temperature oxidation resistance.
Background technology
Graphite material has good conduction, thermal conductivity and good chemical stability and self lubricity, applied range, but shortcoming is oxidizable while being high temperature.Graphite oxidation is since 450 DEG C, and 750 DEG C of rear oxidations sharply increase, and with temperature rising two aggravations.When oxidational losses is serious, use properties sharply declines.Roller shell taking graphite as material is the key part on cold-reduced silicon sheet furnace roller of continuous annealing furnace, requires operation steady in a long-term under 1200 DEG C of certain moistures, thereby the antioxidant property of graphite material is had higher requirement.
Heat treatment furnace is the key equipment that silicon steel is produced, and graphite roller shell is the key part in heat treatment furnace.Graphite roller shell is installed in heat treatment furnace, and along the direction distribution of moving with steel in stove, vertical with the direction moving with steel, by mechanical transmission roller core driven rotary, steel band thereon surface moves through, and is heat-treated stove and is heated to more than 1000 DEG C together with silicon steel.Be subject to processing requirement and environmental influence, in heat treatment furnace, there is the oxidizing medium such as oxygen, moisture content, these media at high temperature produce serious oxygenizement to graphite roller shell, cause its oxidated and short texture, strength degradation, affects the quality product of silicon steel, life-span and the equipment operating efficiency of roller shell self.
Existing many research about Oxidation Resistance of Graphite Material both at home and abroad, the method that improves its antioxidant property mainly contains 3 kinds: coating, self-healing are legal, pickling process.According to the data that can inquire about and the supplier information of recognizing, the silicon steel thermal treatment furnace graphite roller shell of producing for current China, anti-oxidation tech is mainly to have two classes:
One class is to adopt oxide solution dipping method.By Al
2o
3, SiO
2, TiO
2make ultrafine powder or micro mist Deng the non-oxidized substance such as oxide compound or SiC, routine stable dispersion is made colloidal solution in solution according to a certain ratio.Then with vacuum pressed dipping method, oxide solution is immersed to graphite roller shell matrix.Through in after high-temperature heat treatment, in graphite matrix surface and pore, form ceramic protective film.O will be contained with this in environment for use (process furnace)
2, H
2the matrix graphite material of the gas of the oxydised components such as O and graphite roller shell separates, and is enclosed within the object of resisting oxidation, wear resistance in hot environment thereby reach raising graphite roller.
Another kind is to adopt phosphate solution dipping method.Select some phosphate solutions, if aluminium dihydrogen phosphate, primary magnesium phosphate (sodium) etc. are as soaker, oxide solution is immersed to graphite roller shell matrix with vacuum pressed dipping method.Through in after high-temperature heat treatment, make it at high temperature be converted into a material such as metaphosphate, pyrophosphate salt being tied to.
Form theory according to glass, [the PO in these phosphoric acid salt
4] be phosphorus oxygen tetrahedral structure, be the basic structural unit that forms phosphorus oxygen glass, be laminate structure, between layer, be to be maintained together by Van der Waals force.Taking sodium phosphate salt as example, work as P
2o
5in melt, add Na
2when O, phosphorus oxygen glass structure will change chain into from stratiform, be to be combined by Na-O ionic linkage between chain, make structure more be tending towards strong, and thermostability and chemical stability thereof are improved, thereby have better antioxidant effect than simple phosphate impregnation.
Therefore, adopt phosphoric acid salt dipping, in stopping up graphite roller shell matrix pore, form one deck viscosity protective membrane at the pore inwall of matrix, will in environment for use (process furnace), contain O
2, H
2the gas of the oxydised components such as O and matrix graphite material separate, and are enclosed within the object of resisting oxidation, wear resistance in hot environment thereby reach raising graphite roller.
From practical effect, these methods have improved the resistance of oxidation of graphite roller shell to a certain extent.But, due to these dipping solutions and with the inherent characteristics of graphite material combination, adopt the graphite roller shell of making in this way and support for a long time oxidation resistant temperature below 900 DEG C, the anti-oxidant test-results in application practice and laboratory further shows, the graphite roller shell that this mode is made is the difficult space that has further raising oxidation resistance temperature.
Summary of the invention
Object of the present invention aims to provide a kind of surface treatment method that improves silicon steel graphite roller shell high temperature oxidation resistance, makes graphite roller cover possess stronger resistance of oxidation.
According to the present invention, a kind of surface treatment method that improves silicon steel graphite roller shell high temperature oxidation resistance is provided, comprise the following steps: step 1, the processing of roller shell matrix surface; Step 2, dip treating; Step 3, intermediate temperature setting processing; Step 4, non-oxidation Pintsch process ceramic.Wherein, roller shell matrix is graphite matrix; The processing of roller shell matrix surface makes anti-oxidant coat be combined better with roller shell matrix; The dipping solution of dip treating is liquid Polycarbosilane; The solidification value of intermediate temperature setting processing is 150～200 DEG C; Non-oxidation cracking ceramic temperature is 1000～1200 DEG C.
According to one embodiment of the invention, after step 4, also comprise following subsequent step: step 5, non-oxidation is cooling; Step 6, roller shell surface finish; Step 7, roller shell finished product packing.
According to one embodiment of the invention, step 1 comprises: step 1.1, roller shell matrix surface texturing processing; Step 1.2, roller shell matrix surface clean.Wherein, roller shell matrix surface texturing processing makes roller shell matrix surface form larger combined surface area, opens as much as possible matrix surface pore; Roller shell matrix surface clean adopts ultrasonic cleaning.
According to one embodiment of the invention, step 2 comprises: step 2.1, roller shell matrix is put into impregnating autoclave; Step 2.2, vacuumizes impregnating autoclave; Step 2.3, injects dipping solution; Step 2.4, impregnating by pressure; Step 2.5, decompression, takes out the roller shell matrix after dipping.Wherein, the concentration of dipping solution is 25～50%; The pressure of impregnating by pressure is 0.5～0.8MPa.
According to one embodiment of the invention, backspace step 2 after step 3 completes, repeatedly.
According to one embodiment of the invention, the vacuum tightness that impregnating autoclave vacuumizes is 0.06～0.09MPa.
According to one embodiment of the invention, the dipping time of impregnating by pressure is 1～2h.
According to one embodiment of the invention, the time of non-oxidation Pintsch process ceramic is 1～2h.
According to one embodiment of the invention, the volume density of roller shell matrix is 1.74g/cm
3, apparent porosity is 14%.
According to one embodiment of the invention, the molecular weight of Polycarbosilane is 2000～2500.
According to one embodiment of the invention, its high temperature oxidation rate of weight loss is 29%～38%.
Adopt technical scheme of the present invention, can change the physicals of graphite roller shell, increased volume density, reduced apparent porosity, the resistance of oxidation of graphite roller shell is improved.
Brief description of the drawings
In the present invention, identical Reference numeral represents identical feature all the time, wherein:
Fig. 1 is the schema that the present invention improves the surface treatment method of silicon steel graphite roller shell high temperature oxidation resistance.
Embodiment
Further illustrate technical scheme of the present invention below in conjunction with drawings and Examples.
Along with the development that China's silicon steel is produced, increase for the demand of pyrographite roller shell, 900 DEG C of following domestic graphite roller shells of oxidation resistance temperature have been difficult to meet this demand.Based on the present situation of above-mentioned domestic graphite roller shell production technology, in order further to improve the antioxidant property of roller shell, improve work-ing life, reduce the production cost of silicon steel, need in the oxidation-resistance treatment technology of graphite roller shell and method, have breakthrough.
The present invention, by graphite roller shell matrix adopting macromolecular material is flooded and pyroprocessing, improves the antioxidant property of these graphite roller shells, improves its work-ing life, and then improves quality product and the throughput of silicon steel.
The present invention adopts a kind of macromolecular material-Polycarbosilane as soaker; graphite matrix to roller shell floods; then pyroprocessing; with the surface at graphite roller shell matrix and the inner a kind of SiC ceramic protective layer that can resist high temperature oxidation effect, the ability of the oxidizing medium high temperature oxidations such as raising graphite roller shell opposing oxygen and moisture content of obtaining.
Polycarbosilane is a kind of high molecular polymer taking Si-C as main chain.Normal temperature have common organic polymer with group, as CH
3, CH
2, Si-CH
2, Si-CH
2the organic groups such as-Si.After pyroprocessing, organic group disappears, and remaining is Si-C class material.This material, the large density of hardness is high, has good high-temperature stability, in the time removing organic group can with graphite in gac atom have good bonding force, wrap on the surface of graphite roller shell, can strengthen its high temperature oxidation resistance.
The route of preparing Polycarbosilane is to adopt dichlorodimethylsilane as initial feed, first makes polydimethyl silane by sodium condensation, then under High Temperature High Pressure, changes Polycarbosilane into.The molecular weight of the product of making is like this 1000～2000, fusing point is 200 degree left and right, soluble in the organic solvents such as toluene, there is good spinning property, and the Polycarbosilane molecular weight that the present invention adopts is 2000～2500, can adopt the organic solvents such as toluene, also can adopt other the common solvent that is applicable to Polycarbosilane.
Moreover, the Polycarbosilane of proper concn, can also be by means of certain dipping method, be penetrated into graphite matrix inside, on coating and basal body interface, form gradient cladding, thereby alleviate the interfacial stress between coating and matrix, improved the bonding strength wrapping between film and matrix, coat and matrix are combined as a whole better.
As shown in Figure 1, method of the present invention mainly comprises following flow process:
Step 1: the processing of roller shell matrix surface, for coat and matrix are combined as a whole better.
Step 1.1: first need the graphite roller shell matrix surface of moulding to carry out texturing processing, make roller shell matrix surface form larger combined surface area, open as much as possible matrix surface pore.
Step 1.2: roller shell matrix surface clean, adopts ultrasonic technology to clean.
Step 2: dip treating.Impregnated graphite matrix adopting be liquid Polycarbosilane.
Step 2.1: roller shell matrix is put into impregnating autoclave.
Step 2.2: impregnating autoclave is vacuumized to vacuum tightness 0.06～0.09MPa.
Step 2.3: inject dipping solution.According to experimental result, the concentration of solution is controlled at 25～50%, the immersion depth maximum in graphite matrix, and the oxidation-resistance of graphite roller shell finished product is best.
Step 2.4: impregnating by pressure.After in steeping fluid injects impregnating autoclave, be forced into 0.5～0.8MPa, steeping fluid is entered in the pore of graphite matrix as much as possible.
Step 2.5: decompression, take out the roller shell matrix after dipping.
Step 3: intermediate temperature setting processing.Base material after dipping is cured in warm environment after taking out in 150～200 DEG C.
As a kind of preferred implementation of the present invention, above-mentioned step 3, after completing, can optionally be returned to step 2 again, then carry out single-steeping processing, and so repeatable operation repeatedly.The number of times of dipping is larger on the impact of antioxidant effect, and relevant with the concentration of steeping fluid, therefore in order to reach different antioxidant effects, can adjust by the concentration of steeping fluid and dipping number of times.
Step 4: non-oxidation Pintsch process ceramic, temperature is 1000～1200 DEG C, this temperature is to require to determine with the experimental result of Si-C ceramic according to the cracking of steeping fluid Polycarbosilane.
Step 5: non-oxidation is cooling.
Step 6: roller shell surface finish.
Step 7: roller shell finished product packing.
Below by 3 embodiment, above-mentioned step and parameter selection are described, for 3 embodiment, parameter area is:
(1) graphite roller shell matrix primary sample: volume density 1.74g/cm
3; Apparent porosity 14%.
(2) impreg: Polycarbosilane liquid; Molecular weight 2000～2500; Concentration 25～50%.
(3) impregnation technology: vacuum tightness 0.06～0.09MPa; Pressure 0.5～0.8MPa; Dipping time 1～2h.
(4) solidification treatment: 150～200 DEG C of temperature.
(5) cracking ceramic: 1000～1200 DEG C of temperature; Time 1～2h.
embodiment 1
Impregnation concentration is 25%, and dipping number of times is 2 times, and through after the surface treatment method of raising silicon steel graphite roller shell high temperature oxidation resistance of the present invention, the volume density of graphite roller shell is 1.82g/cm
3, void content is 7%, high temperature oxidation rate of weight loss is 29(1100 DEG C × 2h).
embodiment 2
Impregnation concentration is 35%, and dipping number of times is 2 times, and through after the surface treatment method of raising silicon steel graphite roller shell high temperature oxidation resistance of the present invention, the volume density of graphite roller shell is 1.79g/cm
3, void content is 8%, high temperature oxidation rate of weight loss is 31(1100 DEG C × 2h).
embodiment 3
Impregnation concentration is 45%, and dipping number of times is 1 time, and through after the surface treatment method of raising silicon steel graphite roller shell high temperature oxidation resistance of the present invention, the volume density of graphite roller shell is 1.81g/cm
3, void content is 11%, high temperature oxidation rate of weight loss is 38(1100 DEG C × 2h).
Above-mentioned experimental result is as shown in the table.
In addition, be 50% embodiment although above-mentioned 3 embodiment do not provide impregnation concentration, 50% impregnation concentration is equally applicable to method of the present invention.And as can be seen from the above table, in the situation that other conditions are constant, the raising of impregnation concentration can reduce the volume density of graphite roller shell, increase void content and high temperature oxidation rate of weight loss.And on the other hand, dipping number of times is larger on the impact of antioxidant effect, even if the concentration of steeping fluid has larger difference, but flood number of times by adjustment, can obtain equally close antioxidant effect.
Can find out by the above embodiments, through the present invention's graphite roller shell after treatment, its Main physical performance changes a lot:
(1) volume density increases.Because steeping fluid immerses pore and is attached to the surface of graphite substrate, and form the ceramic layer of high-compactness, the volume density of graphite substrate is increased;
(2) apparent porosity reduces.Because steeping fluid has formed the ceramic layer with sealing effect in the surface of graphite substrate and pore, the apparent porosity of graphite substrate is reduced greatly;
(3) resistance of oxidation improves.Because graphite substrate surface has formed ceramic layer, the opposing oxygen of graphite roller shell entirety and moisture content high temperature oxidation ability are improved.
Those of ordinary skill in field of the present invention will be appreciated that, above specification sheets is only one or more embodiments in the numerous embodiment of the present invention, and not uses limitation of the invention.Any equalization variation, modification for the above embodiment and be equal to the technical schemes such as alternative, as long as connotation scope according to the invention, all will drop in the scope that claims of the present invention protect.
Claims (11)
1. a surface treatment method that improves silicon steel graphite roller shell high temperature oxidation resistance, is characterized in that, comprises the following steps:
Step 1, the processing of roller shell matrix surface;
Step 2, dip treating;
Step 3, intermediate temperature setting processing;
Step 4, non-oxidation Pintsch process ceramic;
Wherein, described roller shell matrix is graphite matrix; The processing of described roller shell matrix surface makes anti-oxidant coat be combined better with roller shell matrix; The dipping solution of described dip treating is liquid Polycarbosilane; The solidification value of described intermediate temperature setting processing is 150～200 DEG C; Described non-oxidation cracking ceramic temperature is 1000～1200 DEG C.
2. the surface treatment method of raising silicon steel graphite roller shell high temperature oxidation resistance as claimed in claim 1, is characterized in that, after step 4, also comprises following subsequent step:
Step 5, non-oxidation is cooling;
Step 6, roller shell surface finish;
Step 7, roller shell finished product packing.
3. the surface treatment method of raising silicon steel graphite roller shell high temperature oxidation resistance as claimed in claim 1, is characterized in that, described step 1 comprises:
Step 1.1, roller shell matrix surface texturing processing;
Step 1.2, roller shell matrix surface clean;
Wherein, described roller shell matrix surface texturing processing makes roller shell matrix surface form larger combined surface area, opens as much as possible matrix surface pore; Described roller shell matrix surface clean adopts ultrasonic cleaning.
4. the surface treatment method of raising silicon steel graphite roller shell high temperature oxidation resistance as claimed in claim 1, is characterized in that, described step 2 comprises:
Step 2.1, puts into impregnating autoclave by roller shell matrix;
Step 2.2, vacuumizes impregnating autoclave;
Step 2.3, injects dipping solution;
Step 2.4, impregnating by pressure;
Step 2.5, decompression, takes out the roller shell matrix after dipping;
Wherein, the concentration of described dipping solution is 25～50%; The pressure of described impregnating by pressure is 0.5～0.8MPa.
5. the surface treatment method of raising silicon steel graphite roller shell high temperature oxidation resistance as claimed in claim 1, is characterized in that, backspace step 2 after described step 3 completes, repeatedly.
6. the surface treatment method of raising silicon steel graphite roller shell high temperature oxidation resistance as claimed in claim 4, is characterized in that, the vacuum tightness that described impregnating autoclave vacuumizes is 0.06～0.09MPa.
7. the surface treatment method of raising silicon steel graphite roller shell high temperature oxidation resistance as claimed in claim 4, is characterized in that, the dipping time of described impregnating by pressure is 1～2h.
8. the surface treatment method of raising silicon steel graphite roller shell high temperature oxidation resistance as claimed in claim 1, is characterized in that, the time of non-oxidation Pintsch process ceramic is 1～2h.
9. the surface treatment method of raising silicon steel graphite roller shell high temperature oxidation resistance as claimed in claim 1, is characterized in that, the volume density of described roller shell matrix is 1.74g/cm
3, apparent porosity is 14%.
10. the surface treatment method of raising silicon steel graphite roller shell high temperature oxidation resistance as claimed in claim 1, is characterized in that, the molecular weight of described Polycarbosilane is 2000～2500.
The surface treatment method of 11. raising silicon steel graphite roller shell high temperature oxidation resistances as claimed in claim 1, is characterized in that, its high temperature oxidation rate of weight loss is 29%～38%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115707A (en) * | 2016-06-29 | 2016-11-16 | 武汉科技大学 | A kind of antioxidative crystalline flake graphite powder body and preparation method thereof |
| CN106977231A (en) * | 2017-03-31 | 2017-07-25 | 华东理工大学 | A kind of processing method of new raising carbon material antioxygenic property |
| CN108975956A (en) * | 2018-08-31 | 2018-12-11 | 武汉钢铁有限公司 | Improve the method that silicon steel continuous annealing furnace covers antioxygenic property with medium temperature charcoal |
| CN113698232A (en) * | 2021-08-19 | 2021-11-26 | 武汉钢铁有限公司 | Low-temperature carbon sleeve resistant to ammonia gas corrosion and abrasion and production method thereof |
| CN116462530A (en) * | 2022-01-12 | 2023-07-21 | 宝山钢铁股份有限公司 | Phosphorus-free impregnation method of graphite roller sleeve |
-
2013
- 2013-03-15 CN CN201310082485.9A patent/CN104045376B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| 付志强等: "PCS先驱体转化法制备SiC涂层的浸渍工艺", 《材料工程》, no. 3, 31 December 2003 (2003-12-31), pages 28 - 30 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115707A (en) * | 2016-06-29 | 2016-11-16 | 武汉科技大学 | A kind of antioxidative crystalline flake graphite powder body and preparation method thereof |
| CN106977231A (en) * | 2017-03-31 | 2017-07-25 | 华东理工大学 | A kind of processing method of new raising carbon material antioxygenic property |
| CN108975956A (en) * | 2018-08-31 | 2018-12-11 | 武汉钢铁有限公司 | Improve the method that silicon steel continuous annealing furnace covers antioxygenic property with medium temperature charcoal |
| CN108975956B (en) * | 2018-08-31 | 2021-05-18 | 武汉钢铁有限公司 | Method for improving oxidation resistance of medium-temperature carbon sleeve for silicon steel continuous annealing furnace |
| CN113698232A (en) * | 2021-08-19 | 2021-11-26 | 武汉钢铁有限公司 | Low-temperature carbon sleeve resistant to ammonia gas corrosion and abrasion and production method thereof |
| CN116462530A (en) * | 2022-01-12 | 2023-07-21 | 宝山钢铁股份有限公司 | Phosphorus-free impregnation method of graphite roller sleeve |
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| CN104045376B (en) | 2016-03-30 |
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