CN101659550B - Method for preparing metal impregnation carbon/graphite material - Google Patents
Method for preparing metal impregnation carbon/graphite material Download PDFInfo
- Publication number
- CN101659550B CN101659550B CN2009100754510A CN200910075451A CN101659550B CN 101659550 B CN101659550 B CN 101659550B CN 2009100754510 A CN2009100754510 A CN 2009100754510A CN 200910075451 A CN200910075451 A CN 200910075451A CN 101659550 B CN101659550 B CN 101659550B
- Authority
- CN
- China
- Prior art keywords
- temperature
- powder
- carbon
- graphite powder
- under
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Ceramic Products (AREA)
Abstract
A method for preparing metal impregnation carbon/graphite material is as follows: 60 to 70wt% of calcined coke, 25 to 35wt% of artificial graphite powder and 5 to 10wt% of natural graphite powder are fully and evenly mixed in a mixer and preheated to 120 to 150 DEG C, thus obtaining mixed filler; binder pitch of the softening point of 90 to 120 DEG C and the residual carbon rate of 48 to 55wt% is heated and melted, then the mixed filler is added, and the mixed filler and the binder pitch are mixed for 1 to 3h at the temperature of 120 to 150 DEG C, after mixing, sheet rolling is carried out for 6 to 10 times at the temperature of 120 to 150 DEG C, and the thickness of the rolled plate is less than 1mm, after cooling, the rolled plate is smashed to less than 200Mu m, thus preparing the final pressed powder; the pressed powder is molded and pressed at 60 to 100MPa and then is put into a carbonization furnace at inert atmosphere and heated to 1300 to 1350 DEG C at the heating rate of 5 to 10 DEG C/h, and the constant temperature is kept for 1 to 2h at the highest temperature; and the material is naturally cooled to less than 100 DEG C and is taken out of the furnace, thus obtaining the material. The method has the advantages of high mechanical strength, small aperture and uniform distribution.
Description
Technical field
The invention belongs to a kind of preparation method of metal impregnation carbon/graphite substrate material.
Background technology
Carbon/graphite material has good self-lubricating property, and frictional coefficient is little, and linear expansivity is low, thereby in industry, is widely used as machinery sealing material.But general carbon/graphite material charing sintering forms the little (1.4～1.5g/cm of back volume density
3), low, the short texture (the internal openings rate reaches 20～30%) of intensity, be difficult to the machinery sealing material as high PV (pressure and rotating speed) value operating mode.If with the said material is matrix, utilize HTHP that other molten metal material is immersed in its open pore, form firm reticulated structure, then can improve its compactness, intensity and wear resistance greatly.The carbon graphite material that soaks metal has higher physical strength (its mechanical property can improve 3～6 times than the matrix carbon/graphite material); Wear resistance and tough preferably; Have the characteristic of graphite and metal concurrently, therefore, the machinery sealing material under the high PV value operating mode; Be after utilizing carbon/graphite material through the molten metal dipping, to be used as machinery sealing material under the high PV value operating mode mostly.
Research shows that for soaking the metal carbon/graphite material, the ideal distribution state of metal in the carbonaceous base substrate is that the fine mesh even structure distributes, and this can not only effectively improve the density reinforcing effect to the carbonaceous base substrate, and helps improving the friction and wear behavior of material; But with regard to the immersion amount; But be not the more the better as the immersion amount of dipping charing organism, this is because the frictional coefficient of metal is generally bigger, though the too big intensity and the opacity that can improve material better of immersion amount; But make the frictional coefficient amplification of material bigger, its tribological property is descended; In addition, because the thermal expansivity of metal is big, frictional coefficient is high, and the submerged metal must be uniformly distributed in the carbon matrix with fine mesh, could effectively improve the tribological property of material.If it is inhomogeneous or local state of aggregation arranged to immerse Metal Distribution in charcoal/graphite matrix; Molten metal is in the cooling curing process; Can in carbon matrix, form uneven internal stress and the coefficient of local friction of matrix material is increased greatly, also can cause its tribological property to reduce significantly; In addition, the local metallic region of assembling is big owing to frictional coefficient, under high slew rope; Surface of friction moment temperature rise is very high, and the fastness serious wear makes the fastness poor surface finish; Its frictional coefficient is increased, and tribological property worsens, and causes the uneven wearing and tearing aggravation of fraction time; Leakage phenomenon is more and more serious, finally causes the sealing element seal failure.Therefore, for charcoal/graphite matrix that metal impregnation is used, the hole size and the even structure degree of control charcoal/graphite substrate material are the keys of final impregnating metal carbon/graphite material mechanical property of decision and tribological property.
Summary of the invention
The preparation method who the purpose of this invention is to provide charcoal/graphite sealing material that a kind of physical strength is high, the aperture is little and be evenly distributed.
M106 charcoal/graphite is that early general machinery sealing material is gone up in industry, also be a kind of matrix of immersion type charcoal/graphite sealing material, but because its bore size is bigger, pore size distribution is irregular, is difficult to satisfy present request for utilization.To M106 carbon/graphite material exposed problems in application process, the present invention overcomes above-mentioned defective through the optimization design to raw material, composition of raw materials and material preparation process.
Preparation process of the present invention comprises the steps:
(1) be that calcined petroleum coke, natural graphite powder and the graphous graphite powder of 10-50 μ m is 60-70wt% by the content of calcined coke at first with median size; Graphous graphite powder is 25-35wt%; Natural graphite powder is that 5-10wt% is preheated to 120-150 ℃ behind the abundant mixing of mixing tank, obtains mixed fillers;
(2) be 90-120 ℃ with softening temperature, after the carbon residue rate is 48-55wt% binder pitch heat fused, adds in the mixed fillers and under 120-150 ℃ of temperature, mix 1-3h that wherein binder pitch accounts for the 30-42wt% of mixed fillers;
(3) mix finish after, under 120-150 ℃ of temperature, roll sheet, rolling the sheet number of times is 6-10 time, the thickness that rolls sheet is crushed to 200 μ m and processes final press-powder after following below 1mm after the cooling;
(4) press-powder after the compression molding, is inserted in the charring furnace of inert atmosphere under 60-100MPa earlier, with the temperature rise rate of 5-10 ℃/h to 1300-1350 ℃, and under top temperature constant temperature 1-2h; Come out of the stove after naturally cooling to below 100 ℃, accomplish the preparation of material.
Its calcining temperature of described calcined petroleum coke is at 1200-1300 ℃.
Described binder pitch is meant the coal tar mid-temperature pitch of modification, and wherein softening temperature is 90-120 ℃, and the carbon residue rate is 48-55wt%.
Advantage of the present invention is following:
Say from raw materials used angle that (1) the present invention does not use the carbonaceous raw material of special qualification, be the general raw material of selling on the market, so raw material Jiao's cost is lower.From preparation technology, do not need special conditions, general carbon element enterprise all can realize.
(2) the M106 machinery sealing material is that main stuffing and excessive pitch are sticker with ultra-fine carbon black (about the about 20nm of median size) in formulating of recipe; Being prone to produce ultrafine particle in the prepared moulding press-powder reunites and the sticker skewness; Even Local enrichment, cause the oversized hole of the uneven ultra micro pore drawn game of generation portion in the final material.The used packing material size size of the present invention is relatively large, is difficult in the mixing process producing reuniting; And also can reduce the local accumulative probability of press-powder medium pitch through optimizing the binder pitch consumption.Also in filler, introduce Graphite Powder 99 in addition, reduced the frictional coefficient of final charcoal/graphite substrate material, improve himself lubricity.
(3) in material prepn process of the present invention; Through repeatedly rolling blade technolgy; Make and be coated on the space that mixed fillers particle surface pitch infiltrates filler grain; Improve the homodisperse degree of pitch in thickener, and prevented that filler from reuniting and the pitch part is gathered, thereby improved the performance and the microtexture of material greatly.
Embodiment
Embodiment 1
At first will be after 1300 ℃ of processing, median size is that calcined petroleum coke and natural graphite powder (median size 15 μ m) and the graphous graphite powder (median size 40 μ m) of 30 μ m is 65wt% by the content of calcined coke; Graphous graphite powder is 28wt%; Natural graphite powder is that 7wt% is behind the abundant mixing of mixing tank; And be poured into and be preheated to 130 ℃ in the kneader, obtain mixed fillers; Be 116 ℃ with softening temperature then, after the carbon residue rate is the binder pitch heat fused of 52.6wt%, pours under 130 ℃ of temperature, to mix in the above-mentioned mixed fillers and pinch 2h that wherein binder pitch accounts for the 40wt% of mixed fillers.After mixing finishes, under 130 ℃ of temperature, roll sheet, rolling the sheet number of times is 6 times, and the thickness that rolls sheet is below 0.9mm.The sheet that to process after the cooling is crushed to the final press-powder of the acquisition of back below the 75 μ m.Compression molding under the 80MPa of above-mentioned press-powder elder generation, molding blank is inserted in the charring furnace of Ar atmosphere, with the temperature rise rate to 1300 of 10 ℃/h ℃, and under top temperature constant temperature 1h; Come out of the stove after naturally cooling to below 100 ℃, accomplish the preparation of material.The basic physicals of final material is seen table 1.
Embodiment 2
At first will be after 1300 ℃ of processing, median size is that calcined petroleum coke and natural graphite powder (median size 13 μ m) and the graphous graphite powder (median size 45 μ m) of 45 μ m is 60wt% by the content of calcined coke; Graphous graphite powder is 32wt%; Natural graphite powder is that 8wt% is behind the abundant mixing of mixing tank; And be poured into and be preheated to 120 ℃ in the kneader, obtain mixed fillers; Be 102 ℃ with softening temperature then, after the carbon residue rate is the binder pitch heat fused of 49.6wt%, pours under 120 ℃ of temperature, to mix in the above-mentioned mixed fillers and pinch 2h that wherein binder pitch accounts for the 38wt% of mixed fillers.After mixing finishes, under 120 ℃ of temperature, roll sheet, rolling the sheet number of times is 7 times, and the thickness that rolls sheet is below 1mm.The sheet that to process after the cooling is crushed to the final press-powder of the acquisition of back below the 200 μ m.Compression molding under the 80MPa of above-mentioned press-powder elder generation, molding blank is inserted in the charring furnace of Ar atmosphere, with the temperature rise rate to 1350 of 8 ℃/h ℃, and under top temperature constant temperature 2h; Come out of the stove after naturally cooling to below 100 ℃, accomplish the preparation of material.The basic physicals of final material is seen table 1.
Embodiment 3
Will be after 1250 ℃ of processing, median size is that calcined petroleum coke and natural graphite powder (median size 11 μ m) and the graphous graphite powder (median size 45 μ m) of 40 μ m is 62wt% by the content of calcined coke; Graphous graphite powder is 32wt%; Natural graphite powder is that 6wt% is behind the abundant mixing of mixing tank; And be poured into and be preheated to 130 ℃ in the kneader, obtain mixed fillers; Be 106 ℃ with softening temperature then, after the carbon residue rate is the binder pitch heat fused of 50.4wt%, pours under 130 ℃ of temperature, to mix in the above-mentioned mixed fillers and pinch 1.5h that wherein binder pitch accounts for the 36wt% of mixed fillers.After mixing finishes, under 130 ℃ of temperature, roll sheet, rolling the sheet number of times is 8 times, and the thickness that rolls sheet is below 0.8mm.The sheet that to process after the cooling is crushed to the final press-powder of the acquisition of back below the 150 μ m.Compression molding under the 100MPa of above-mentioned press-powder elder generation, molding blank is inserted in the charring furnace of Ar atmosphere, with the temperature rise rate to 1300 of 5 ℃/h ℃, and under top temperature constant temperature 2h; Come out of the stove after naturally cooling to below 100 ℃, accomplish the preparation of material.The basic physicals of final material is seen table 1.
Embodiment 4
At first will be after 1200 ℃ of processing, median size is that calcined petroleum coke and natural graphite powder (median size 8 μ m) and the graphous graphite powder (median size 50 μ m) of 30 μ m is 58wt% by the content of calcined coke; Graphous graphite powder is 32wt%; Natural graphite powder is that 10wt% is behind the abundant mixing of mixing tank; And be poured into and be preheated to 125 ℃ in the kneader, obtain mixed fillers; Be 95 ℃ with softening temperature then, after the carbon residue rate is the binder pitch heat fused of 48.6wt%, pours under 125 ℃ of temperature, to mix in the above-mentioned mixed fillers and pinch 2h that wherein binder pitch accounts for the 34wt% of mixed fillers.After mixing finishes, under 125 ℃ of temperature, roll sheet, rolling the sheet number of times is 5 times, and the thickness that rolls sheet is below 0.7mm.The sheet that to process after the cooling is crushed to the final press-powder of the acquisition of back below the 100 μ m.Compression molding under the 60MPa of above-mentioned press-powder elder generation, molding blank is inserted in the charring furnace of Ar atmosphere, with the temperature rise rate to 1300 of 5 ℃/h ℃, and under top temperature constant temperature 2h; Come out of the stove after naturally cooling to below 100 ℃, accomplish the preparation of material.The basic physicals of final material is seen table 1.
Embodiment 5
At first will be after 1250 ℃ of processing, median size is that calcined petroleum coke and natural graphite powder (median size 12 μ m) and the graphous graphite powder (median size 40 μ m) of 35 μ m is 60wt% by the content of calcined coke; Graphous graphite powder is 30wt%; Natural graphite powder is that 10wt% is behind the abundant mixing of mixing tank; And be poured into and be preheated to 120 ℃ in the kneader, obtain mixed fillers; Be 95 ℃ with softening temperature then, after the carbon residue rate is the binder pitch heat fused of 48.6wt%, pours under 120 ℃ of temperature, to mix in the above-mentioned mixed fillers and pinch 3h that wherein binder pitch accounts for the 32wt% of mixed fillers.After mixing finishes, under 120 ℃ of temperature, roll sheet, rolling the sheet number of times is 10 times, and the thickness that rolls sheet is below 0.5mm.The sheet that to process after the cooling is crushed to the final press-powder of the acquisition of back below the 75 μ m.Compression molding under the 80MPa of above-mentioned press-powder elder generation, molding blank is inserted in the charring furnace of Ar atmosphere, with the temperature rise rate to 1350 of 6 ℃/h ℃, and under top temperature constant temperature 1h; Come out of the stove after naturally cooling to below 100 ℃, accomplish the preparation of material.The basic physicals of final material is seen table 1.
The basic physicals that above instance makes material all is listed in the table below:
The basic physicals of table 1 material
| Numbering | Density g/cm 3 | Curved strong MPa | Pressure MPa | Percentage of open area % | Average pore size (μ m) | Shore hardness | Frictional coefficient | Degree of graphitization (%) |
| Embodiment 1 | 1.65 | 47.8 | 109.7 | 11.08 | ?0.73 | 62 | 0.20 | 36.7 |
| Embodiment 2 | 1.63 | 42.8 | 93.7 | 12.31 | ?0.61 | 59 | 0.15 | 40.8 |
| Embodiment 3 | 1.62 | 41.2 | 90.6 | 16.84 | ?0.57 | 58 | 0.18 | 38.4 |
| Embodiment 4 | 1.60 | 37.0 | 88.3 | 16.15 | ?0.38 | 54 | 0.19 | 39.6 |
| Embodiment 5 | 1.59 | 35.0 | 81.2 | 17.55 | ?0.53 | 55 | 0.14 | 41.0 |
Claims (3)
1. the preparation method of a metal impregnation carbon/graphite material is characterized in that comprising the steps:
(1) be that calcined petroleum coke, natural graphite powder and the graphous graphite powder of 10-50 μ m is 60-70wt% by the content of calcined petroleum coke at first with median size; Graphous graphite powder is 25-35wt%; Natural graphite powder is that 5-10wt% is preheated to 120-150 ℃ behind the abundant mixing of mixing tank, obtains mixed fillers;
(2) be 90-120 ℃ with softening temperature, after the carbon residue rate is 48-55wt% binder pitch heat fused, adds in the mixed fillers and under 120-150 ℃ of temperature, mix 1-3h that wherein binder pitch accounts for the 30-42wt% of mixed fillers;
(3) mix finish after, under 120-150 ℃ of temperature, roll sheet, rolling the sheet number of times is 6-10 time, the thickness that rolls sheet is crushed to 200 μ m and processes final press-powder after following below 1mm after the cooling;
(4) press-powder after the compression molding, is inserted in the charring furnace of inert atmosphere under 60-100MPa earlier, with the temperature rise rate of 5-10 ℃/h to 1300-1350 ℃, and under top temperature constant temperature 1-2h; Come out of the stove after naturally cooling to below 100 ℃, accomplish the preparation of material.
2. the preparation method of a kind of metal impregnation carbon/graphite material as claimed in claim 1 is characterized in that its calcining temperature of described calcined petroleum coke is at 1200-1300 ℃.
3. the preparation method of a kind of metal impregnation carbon/graphite material as claimed in claim 1 is characterized in that described binder pitch is the coal tar mid-temperature pitch of modification, and wherein softening temperature is 90-120 ℃, and the carbon residue rate is 48-55wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100754510A CN101659550B (en) | 2009-09-15 | 2009-09-15 | Method for preparing metal impregnation carbon/graphite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100754510A CN101659550B (en) | 2009-09-15 | 2009-09-15 | Method for preparing metal impregnation carbon/graphite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101659550A CN101659550A (en) | 2010-03-03 |
| CN101659550B true CN101659550B (en) | 2012-03-07 |
Family
ID=41787834
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100754510A Active CN101659550B (en) | 2009-09-15 | 2009-09-15 | Method for preparing metal impregnation carbon/graphite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101659550B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2749979C1 (en) * | 2020-12-21 | 2021-06-21 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Волгоградский государственный технический университет" (ВолгГТУ) | Method for producing carbon-graphite composite material |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103332886B (en) * | 2013-05-08 | 2015-03-18 | 房县天龙石墨碳业有限公司 | Anti-oxidation integrated graphite stopper rod |
| CN103408890B (en) * | 2013-07-18 | 2015-04-22 | 常州大学 | Preparation method of Cu/carbon graphite mechanical sealing composite material |
| CN103435967B (en) * | 2013-07-18 | 2015-04-22 | 常州大学 | Preparation method of Al/carbon graphite mechanical seal composite material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4293533A (en) * | 1974-01-31 | 1981-10-06 | Kureha Kagaku Kogyo Kabushiki Kaisha | Method for producing solid carbon material having high flexural strength |
| CN1724474A (en) * | 2005-05-31 | 2006-01-25 | 哈尔滨工业大学 | Asphalt base carbon/carbon composite material for heating structure and its preparation method |
-
2009
- 2009-09-15 CN CN2009100754510A patent/CN101659550B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4293533A (en) * | 1974-01-31 | 1981-10-06 | Kureha Kagaku Kogyo Kabushiki Kaisha | Method for producing solid carbon material having high flexural strength |
| CN1724474A (en) * | 2005-05-31 | 2006-01-25 | 哈尔滨工业大学 | Asphalt base carbon/carbon composite material for heating structure and its preparation method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2749979C1 (en) * | 2020-12-21 | 2021-06-21 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Волгоградский государственный технический университет" (ВолгГТУ) | Method for producing carbon-graphite composite material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101659550A (en) | 2010-03-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101544497B (en) | Production method for composite carbon graphite material | |
| CN101659550B (en) | Method for preparing metal impregnation carbon/graphite material | |
| CN108046803B (en) | High-strength graphite product produced by adding asphalt coke and method | |
| CN101798221A (en) | Fine texture graphite material and preparation method thereof | |
| CN107235728B (en) | Energy-saving production process of prebaked anode | |
| CN107522196A (en) | A kind of superhard isostatic pressing formed graphite and preparation method thereof | |
| CN1994967A (en) | Processing method for dipping graphite carbon envelope with oxide solution | |
| DE2948977A1 (en) | FIREPROOF GRAPHITE FORMING | |
| CN115108833B (en) | Continuous casting graphite material and preparation method thereof | |
| CN107311686A (en) | A kind of novel preparation process of graphite electrode | |
| CN110819842A (en) | Preparation method of formed part based on reduced graphene oxide and copper composite material | |
| CN104860678A (en) | Method for producing ultra-high power graphite electrode through natural graphite | |
| CN100344533C (en) | Process for preparing high strength carbon/graphite material | |
| CN102674869B (en) | Carbon composite material for side wall of lower part of aluminium electrolysis cell and preparation method thereof | |
| KR20120131705A (en) | Manufacturing method of graphite block | |
| CN113816738A (en) | By using nano TiO2Preparation of graphite material with ultrahigh conductive hot isostatic pressure and method thereof | |
| CN107473745A (en) | A kind of preparation method of water lubriucated bearing impregnated graphite materials | |
| CN116496087B (en) | Superfine structure special carbon material and preparation method thereof | |
| CN114804876B (en) | Preparation method of high-wear-resistance end face sealing graphite material | |
| CN101985760B (en) | Components of graphitized anode and preparation method thereof | |
| CN106673657A (en) | Special carbon material and production method thereof | |
| CN111269021B (en) | Copper-iron-carbon composite sliding plate and preparation method and application thereof | |
| CN110318012A (en) | A kind of self-lubricating nickel-based composite and preparation method thereof | |
| CN102290141A (en) | Method for producing closed paste with waste carbon anode green blocks | |
| CN113213936B (en) | Preparation method of ceramic powder doped modified self-sintered graphite composite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |