CN115815597A - Hard alloy burning-back device and hard alloy burning-back method - Google Patents
Hard alloy burning-back device and hard alloy burning-back method Download PDFInfo
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- CN115815597A CN115815597A CN202211350045.2A CN202211350045A CN115815597A CN 115815597 A CN115815597 A CN 115815597A CN 202211350045 A CN202211350045 A CN 202211350045A CN 115815597 A CN115815597 A CN 115815597A
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- 238000000034 method Methods 0.000 title claims abstract description 37
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- 229910002804 graphite Inorganic materials 0.000 claims abstract description 30
- 239000010439 graphite Substances 0.000 claims abstract description 30
- 238000012856 packing Methods 0.000 claims abstract description 27
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 17
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 14
- 239000000945 filler Substances 0.000 claims abstract description 12
- 239000004575 stone Substances 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims description 26
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- 238000005261 decarburization Methods 0.000 description 19
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Abstract
The invention discloses a hard alloy burning device and a hard alloy burning method. The hard alloy back-burning device comprises: the stone ink box is used for containing the hard alloy to be burned back; the packing layer is filled in a gap between the periphery of the hard alloy to be sintered and the graphite box shell; wherein the filler layer is made of Al 2 O 3 Powder and TiO 2 Powder is mixed and filled, the Al is 2 O 3 20-95% of powder and the balance of TiO 2 And (3) powder. Through verification, the carburization degree of the hard alloy treated by the hard alloy burning device and the hard alloy burning method is obviously reduced, the magnetic saturation is obviously reduced, and the bending strength is obviously improved.
Description
Technical Field
The invention relates to the technical field of hard alloy, in particular to the technical field of eliminating free carbon structures in hard alloy, and specifically relates to a hard alloy burning device and a hard alloy burning method.
Background
The hard alloy is an alloy material prepared by a powder metallurgy process, has a series of excellent properties such as high hardness, wear resistance, good strength and toughness, heat resistance, corrosion resistance and the like, and is widely applied to cutter materials. The hard alloy can be used for cutting cast iron, nonferrous metals, plastics, chemical fibers, graphite, glass, stone and common steel, and can also be used for cutting heat-resistant steel, stainless steel, high manganese steel, tool steel and other materials which are difficult to process.
In the production process of hard alloy, the control requirement of the carbon content of the alloy is extremely high, particularly for the matching of carbon preparation and sintering process, the carbon content of the alloy is always the core of the quality control of hard alloy production enterprises and is most difficult to be stabilized, and free carbon tissues (namely carburization) with different degrees appear after sintering of hard alloy products are often caused by raw material fluctuation, abnormal sintering furnace and mismatching process, so that the performance of the hard alloy is sharply reduced, the use value is basically not high, and further, batch unqualified products are generated, and huge economic loss is caused. For this reason, it is necessary to adopt a method of removing the free carbon structure (i.e., decarburization) in the cemented carbide to change waste into valuable.
The existing decarburization methods mainly comprise the following two methods: the first decarburization method is a reverse sintering method, in which cemented carbide with an excessive free carbon structure is placed in alumina and heated in a hydrogen furnace by using the hydrogen decarburization effect to perform repeated sintering treatment. The other decarburization method is to heat the hard alloy with the excessive free carbon structure in a vacuum furnace and then carry out inert gas quick cooling, and the decarburization method has good decarburization effect but higher cost and is difficult to be used on a large scale.
Disclosure of Invention
The invention mainly aims to provide a hard alloy burning device and a hard alloy burning method, and aims to solve the technical problem that a decarburization method in the prior art is poor in decarburization effect.
In order to achieve the above object, according to a first aspect of the present invention, there is provided a cemented carbide reflow apparatus, comprising:
hard alloy burns device again includes: the stone ink box is used for containing the hard alloy to be burned back; the packing layer is filled in a gap between the periphery of the hard alloy to be sintered and the graphite box shell; wherein the filler layer is made of Al 2 O 3 Powder and TiO 2 Powder is mixed and filled, the Al is 2 O 3 20-95% of powder and the balance of TiO 2 And (3) powder.
As a further improvement of the first aspect of the invention, said Al 2 O 3 The granularity of the powder is 20-100 mu m; the TiO is 2 The particle size of the powder is 10-80 μm.
As a further improvement of the first aspect of the invention, said Al 2 O 3 The granularity of the powder is 50-80 mu m; the TiO is 2 The particle size of the powder is 30-60 mu m.
As a further improvement of the first aspect of the invention, the thickness of the packing layer is more than or equal to 2mm.
As a further improvement of the first aspect of the present invention, the cemented carbide to be sintered is cylindrical or flat; when the diameter or the thickness of the hard alloy to be re-sintered is more than or equal to 4mm and less than 10mm, the thickness of the packing layer is more than or equal to 4mm; when the diameter or the thickness of the hard alloy to be sintered is more than or equal to 10mm and less than 30mm, the thickness of the packing layer is more than or equal to 6mm; when the diameter or the thickness of the hard alloy to be re-sintered is more than or equal to 30mm, the thickness of the packing layer is more than or equal to 8mm.
As a further improvement of the first aspect of the invention, said Al 2 O 3 20-95% of powder and the balance of TiO 2 And (3) powder.
As a further development of the first aspect of the invention, a graphite cover plate fitted with the graphite box is also included.
In order to achieve the above object, according to a second aspect of the present invention, there is provided a cemented carbide re-sintering method, comprising:
the hard alloy burning method comprises the following steps:
(1) Obtaining a graphite box matched with the size of the hard alloy to be re-sintered;
(2) Laying mixed powder at the bottom of the graphite box, and then compacting;
(3) Putting the hard alloy to be sintered;
(4) Continuously laying the mixed powder to ensure that the periphery and the upper part of the hard alloy to be re-sintered are filled with the mixed powder, and then compacting;
(5) Putting the graphite box into a sintering furnace for sintering;
the mixed powder is made of Al 2 O 3 Powder and TiO 2 Powder of Al 2 O 3 20-95% of powder and the balance of TiO 2 And (3) powder.
As a further improvement of the second aspect of the invention, the compaction is carried out with a pressing force of 4 to 8kg/m 3 。
As a further improvement of the second aspect of the present invention, the graphite box is sintered by a sintering process for preparing a cemented carbide to be sintered.
The invention has the following advantages:
first, the filler layer is composed of metal oxide powder, and therefore, the metal oxide absorbs a certain amount of oxygen on the one hand, and on the other hand, combined oxygen at high temperature can undergo redox reaction with carbon. Therefore, the metal oxide filler layer covers the surface of the hard alloy with the free carbon structure, and in the high-temperature sintering process, the free carbon is eliminated by oxygen provided by the filler layer through diffusion and oxidation-reduction reaction, so that the effect of eliminating the free carbon structure is achieved.
Next, the purpose of decarburization is to remove the free carbon structure in the cemented carbide, but bound carbon, which is beneficial to the performance thereof, is also present in the cemented carbide, and when the bound carbon is large, the toughness strength of the cemented carbide is improved. With Al 2 O 3 Powder phase ratio, tiO 2 The oxygen diffusion and redox reaction with free carbon in the powder is more intense, for products with slight degree of free carbon, tiO 2 The powder is easy to cause the condition that the combined carbon of the hard alloy is excessively removed due to excessive burning, and the toughness and the strength of the hard alloy are further influenced. Therefore, the packing layer of the invention is prepared from Al with a certain proportion 2 O 3 Powder and TiO 2 Powder composition of Al 2 O 3 Powder and TiO 2 The mutual cooperation of the powder can ensure the decarbonization effect of free carbon and prevent the bonded carbon from being removed, and finally the proper decarbonization degree is achieved, thereby ensuring the performance of the hard alloy.
In addition, the graphite box made of graphite can support the hard alloy to be re-burnt at high temperature by maintaining high strength, can adsorb free carbon, and is beneficial to the decarburization reaction of the hard alloy at high temperature.
Furthermore, by applying proper compaction treatment to the metal oxide, the metal oxide can be fully and tightly contacted with the hard alloy to be sintered, and the air permeability in the high-temperature sintering process can be ensured, so that the decarburization reaction is carried out to eliminate free carbon. Meanwhile, through compaction treatment and shielding of the graphite cover plate, the metal oxide powder can be prevented from escaping due to vacuumizing in the process of burning, so that the decarburization effect is influenced and the sintering equipment is polluted.
Through verification, the carburization degree of the hard alloy treated by the hard alloy burning device and the hard alloy burning method is obviously reduced, the magnetic saturation is obviously reduced, and the bending strength is obviously improved.
The invention is further described with reference to the following figures and detailed description. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to assist in understanding the invention, and are included to explain the invention and their equivalents and not limit it unduly. In the drawings:
fig. 1 is a schematic structural diagram of a specific embodiment of the cemented carbide reverse sintering apparatus according to the present invention.
The relevant references in the above figures are:
100-hard alloy to be sintered, 200-stone ink box, 300-filler layer and 400-graphite cover plate.
Detailed Description
The invention will be described more fully hereinafter with reference to the accompanying drawings. Those skilled in the art will be able to practice the invention based on these descriptions. Before the present invention is described in detail with reference to the accompanying drawings, it is to be noted that:
the technical solutions and features provided in the present invention in the respective sections including the following description may be combined with each other without conflict.
Moreover, the embodiments of the present invention described in the following description are generally only some embodiments of the present invention, and not all embodiments. Therefore, all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without making creative efforts shall fall within the protection scope of the present invention.
With respect to terms and units in the present invention. The terms "comprising," "having," and any variations thereof in the description and claims of this invention and the related sections are intended to cover non-exclusive inclusions.
Fig. 1 is a schematic structural diagram of a specific embodiment of the cemented carbide reverse sintering apparatus according to the present invention.
As shown in fig. 1, the cemented carbide re-firing device of the present invention comprises a graphite cartridge 200, a filler layer 300, and a graphite cover plate 400. The stone ink box 200 is used for containing the hard alloy 100 to be burned back. The packing layer 300 is filled in the gap between the periphery of the hard alloy 100 to be sintered and the shell of the graphite box 200, and the packing layer 300 is made of Al 2 O 3 Powder and TiO 2 Powder is mixed and filled, the Al is 2 O 3 The mass fraction of the powder is 20-95%, preferably 20-83%, and the balance is TiO 2 And (3) powder. The graphite cover plate 400 is fitted to the graphite cartridge 200.
The Al is 2 O 3 The particle size of the powder is 20-100 μm, preferably 50-80 μm; the TiO is 2 The particle size of the powder is 10 to 80 μm, preferably 30 to 60 μm. When the particle size is larger than the above range, the packing layer 300 may not contact the hard alloy 100 to be sintered uniformly, and when the particle size is smaller than the above range, the packing layer is expensive and has poor permeability due to dense packing, so that the decarburization effect may be affected by too high and too low particle sizes. When Al is present 2 O 3 The particle size of the powder is 50-80 mu m, tiO 2 When the particle size of the powder is 30 to 60 μm, the optimum decarburization effect can be obtained and the material cost is low.
The thickness of the packing layer 300 is more than or equal to 2mm, so that the metal oxide in the packing layer 300 can provide enough oxygen to perform oxidation-reduction reaction with the free carbon in the hard alloy 100 to be re-fired, and the decarburization effect is ensured.
The hard alloy to be sintered is cylindrical or flat; when the diameter or the thickness of the hard alloy to be sintered is more than or equal to 4mm and less than 10mm, the thickness of the packing layer is more than or equal to 4mm; when the diameter or the thickness of the hard alloy to be sintered is more than or equal to 10mm and less than 30mm, the thickness of the packing layer is more than or equal to 6mm; when the diameter or the thickness of the hard alloy to be sintered is more than or equal to 30mm, the thickness of the packing layer is more than or equal to 8mm.
The specific implementation mode of the hard alloy back-burning method provided by the invention is that the hard alloy back-burning device is adopted, and the method specifically comprises the following steps:
(1) Obtaining a graphite box 200 matched with the size of the hard alloy 100 to be sintered;
(2) Laying mixed powder at the bottom of the graphite box 200, and then compacting;
(3) Putting the hard alloy to be re-sintered 100;
(4) Continuously laying the mixed powder to ensure that the mixed powder is filled around and above the hard alloy 100 to be sintered, and then compacting and covering a graphite cover plate 400;
(5) Putting the stone ink box 200 into a sintering furnace for sintering;
the pressing force adopted by the compaction is preferably 4-8 kg/m 3 . When the pressing force is higher than 8kg/m 3 In the process, the metal oxide mixed powder is stacked to form a dense packing layer 300, which affects air permeability and is not favorable for decarburization. When the pressing force is lower than 4kg/m 3 In the process, on one hand, the metal oxide mixed powder is easy to dissipate under the action of vacuum pumping, so that the metal oxide mixed powder cannot uniformly and completely cover the periphery of the hard alloy to be burned back 100, and on the other hand, the hard alloy to be burned back 100 is easy to contact with the graphite box 200 under the action of self weight, so that the carburization hazard is aggravated.
The sintering process for preparing the hard alloy 100 to be sintered is adopted to sinter the graphite box 200, so that the hardness, the grain size and the like of the hard alloy 100 to be sintered can be prevented from being deteriorated due to the sintering, the hard alloy can be sintered together with the product, and the sintering without separately opening a furnace is not needed.
The advantageous effects of the present invention are illustrated below by specific examples.
TABLE 1
The raw material ratios of the packing layers and the thicknesses of the packing layers of examples 1 to 10 are shown in Table 1. The pressing force was the same in examples 1-10, and the sintering processes used were all those of the corresponding cemented carbide to be back-fired.
Examples 1 to 3 differ only inIn Al 2 O 3 And TiO 2 Are different in particle size. As can be seen from the performance data, the particle sizes are too large and too small, which is not favorable for the re-sintering modification.
Example 1 differs from example 4 only in the TiO content of the filler layer 2 The ratio of (a) to (b) is different. As can be seen from the performance data, the TiO increase was modest 2 The proportion of (A) can improve the effect of burning again.
The carburization degree was improved in examples 5 to 6 as compared with examples 1 and 4, and TiO was increased correspondingly 2 The proportion of (A) and (B) achieves better burning effect. Therefore, aiming at different carburization degrees, the adaptive filler proportion needs to be matched, and when the carburization degree is higher, tiO can be increased 2 The ratio of (a) to (b).
Example 7 differs from example 8 in the thickness of the filler layer. By comparison, the magnetic saturation decrease range and the bending strength increase range of the example 8 are small, and the free carbon is not completely eliminated, which shows that the hard alloy to be sintered is very unfavorable for sintering when the diameter of the hard alloy to be sintered is large and the thickness of the filler layer is too thin.
As is clear from comparison of examples 7, 9 and 10, al is contained only 2 O 3 The decarbonization effect of the formed packing layer is poor, and pure TiO2 can cause that the combined carbon which is beneficial to the material performance is adsorbed while free carbon is eliminated, so that the performances such as strength and the like are not improved, and the corresponding reverse burning effect cannot be achieved.
As can be seen from Table 1, the cemented carbide treated by the present invention has reduced magnetic saturation, significantly improved bending strength, stable coercivity and hardness (no deterioration of performance), and significantly reduced carburization, and thus the present invention has excellent decarburization effect, especially when Al is treated by the present invention 2 O 3 The particle size of the powder is 50-80 mu m, tiO 2 The particle size of the powder is 30-60 mu m, al 2 O 3 When the mass fraction of the powder is 20-83%, the packing layer with a certain thickness can obtain the best decarburization effect.
The test method of the magnetic saturation is a standard test method for measuring GB/T23369-2009 hard alloy Magnetic Saturation (MS).
The method for testing the coercive force is GB/T3848-2017 method for measuring the coercive force (magnetic force) of the hard alloy.
The test method of the hardness is 'GB/T7997-2014 hard alloy Vickers hardness test method'.
The testing method of the bending strength is GB/T3851-2015 method for measuring transverse breaking strength of hard alloy.
The testing method of the carburization degree is GB _ T3489-2015 metallographic determination of porosity and amorphous carbon of the hard alloy.
The contents of the present invention have been explained above. Those skilled in the art will be able to implement the invention based on these teachings. All other embodiments, which can be derived by a person skilled in the art from the above description without inventive step, shall fall within the scope of protection of the present invention.
Claims (10)
1. Hard alloy burns device again, its characterized in that: the method comprises the following steps:
the stone ink box is used for containing the hard alloy to be burned back;
the packing layer is filled in a gap between the periphery of the hard alloy to be sintered and the graphite box shell;
wherein the filler layer is made of Al 2 O 3 Powder and TiO 2 Powder is mixed and filled, the Al is 2 O 3 20-95% of powder and the balance of TiO 2 And (3) powder.
2. The cemented carbide reverse firing apparatus as set forth in claim 1, wherein: the Al is 2 O 3 The granularity of the powder is 20-100 mu m; the TiO is 2 The particle size of the powder is 10-80 μm.
3. The cemented carbide reverse firing apparatus as set forth in claim 2, wherein: the Al is 2 O 3 The particle size of the powder is 50 ℃ to80 μm; the TiO is 2 The particle size of the powder is 30-60 μm.
4. The cemented carbide burnback apparatus of claim 1, wherein: the thickness of the packing layer is more than or equal to 2mm.
5. The cemented carbide reverse firing apparatus as set forth in claim 4, wherein: the hard alloy to be sintered is cylindrical or flat; when the diameter or the thickness of the hard alloy to be re-sintered is more than or equal to 4mm and less than 10mm, the thickness of the packing layer is more than or equal to 4mm; when the diameter or the thickness of the hard alloy to be re-sintered is more than or equal to 10mm and less than 30mm, the thickness of the packing layer is more than or equal to 6mm; when the diameter or the thickness of the hard alloy to be sintered is more than or equal to 30mm, the thickness of the packing layer is more than or equal to 8mm.
6. The cemented carbide reverse firing apparatus as set forth in claim 1, wherein: the Al is 2 O 3 The mass fraction of the powder is 20-95%, and the rest is TiO 2 And (3) powder.
7. The cemented carbide reverse firing apparatus as set forth in claim 1, wherein: and the graphite cover plate is matched with the graphite box.
8. The hard alloy burning method comprises the following steps:
(1) Obtaining a graphite box matched with the size of the hard alloy to be sintered;
(2) Laying mixed powder at the bottom of the graphite box, and then compacting;
(3) Putting the hard alloy to be sintered;
(4) Continuously laying the mixed powder to ensure that the periphery and the upper part of the hard alloy to be re-sintered are filled with the mixed powder, and then compacting;
(5) Putting the graphite box into a sintering furnace for sintering;
the mixed powder is made of Al 2 O 3 Powder and TiO 2 Powder of Al 2 O 3 20-95% of powder and the balance of TiO 2 And (3) powder.
9. The cemented carbide reflow method of claim 8, wherein: the pressing force adopted by the compaction is 4-8 kg/m 3 。
10. The cemented carbide reflow method of claim 8, wherein: sintering the graphite box by adopting a sintering process for preparing the hard alloy to be sintered.
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| JPH07242958A (en) * | 1994-03-07 | 1995-09-19 | Toshiba Tungaloy Co Ltd | Composition for powder metallurgy and its production |
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| CN105154818A (en) * | 2015-10-12 | 2015-12-16 | 株洲硬质合金集团有限公司 | Method for eliminating hard alloy carburization defect and paint used in method |
| CN108677136A (en) * | 2018-05-28 | 2018-10-19 | 株洲硬质合金集团有限公司 | A method of eliminating hard alloy decarburization defect |
| CN109576637A (en) * | 2018-12-20 | 2019-04-05 | 株洲硬质合金集团有限公司 | A kind of method for carburizing of hard alloy |
| CN111172372A (en) * | 2020-01-15 | 2020-05-19 | 晋城鸿刃科技有限公司 | Method for processing hard alloy carburized product |
| CN115074568A (en) * | 2022-06-29 | 2022-09-20 | 株洲金韦硬质合金有限公司 | Preparation method of hard alloy with controllable cobalt phase gradient structure |
-
2022
- 2022-10-31 CN CN202211350045.2A patent/CN115815597A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07242958A (en) * | 1994-03-07 | 1995-09-19 | Toshiba Tungaloy Co Ltd | Composition for powder metallurgy and its production |
| CN101921975A (en) * | 2010-05-20 | 2010-12-22 | 长沙华信合金机电有限公司 | Production process for removing non-compound carbon phase in hard alloy |
| CN105154818A (en) * | 2015-10-12 | 2015-12-16 | 株洲硬质合金集团有限公司 | Method for eliminating hard alloy carburization defect and paint used in method |
| CN108677136A (en) * | 2018-05-28 | 2018-10-19 | 株洲硬质合金集团有限公司 | A method of eliminating hard alloy decarburization defect |
| CN109576637A (en) * | 2018-12-20 | 2019-04-05 | 株洲硬质合金集团有限公司 | A kind of method for carburizing of hard alloy |
| CN111172372A (en) * | 2020-01-15 | 2020-05-19 | 晋城鸿刃科技有限公司 | Method for processing hard alloy carburized product |
| CN115074568A (en) * | 2022-06-29 | 2022-09-20 | 株洲金韦硬质合金有限公司 | Preparation method of hard alloy with controllable cobalt phase gradient structure |
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