CN115745612B - Ti 3 SiC 2 Multi-phase composite ceramic wire guide and preparation method thereof - Google Patents
Ti 3 SiC 2 Multi-phase composite ceramic wire guide and preparation method thereof Download PDFInfo
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Abstract
The invention provides a Ti 3 SiC 2 The preparation method of the multi-phase composite ceramic wire guide comprises the following steps: step S1, ti is mixed with 3 SiC 2 Mixing and dispersing the powder master batch and the additive powder to obtain composite powder; s2, mixing the composite powder and an organic binder in a heating mixing internal mixer, crushing the mixed materials, and granulating in a granulator to obtain injection granulating materials; s3, performing injection molding on the injection granulated material to obtain a composite ceramic wire guide green body; s4, placing the composite ceramic wire guide blank body into a degreasing furnace for thermal degreasing to obtain a composite ceramic wire guide biscuit; step S5, heating the composite ceramic biscuit in a vacuum environment, and preserving heat at 1500-1600 ℃ for 30-150min to obtain a sintered body; step S6, placing the sintered body in a hot isostatic pressing furnace, and performing hot isostatic pressing treatment at 1450-1550 ℃ and 100-150MPa for 60-180min to obtain the Ti 3 SiC 2 A multi-phase composite ceramic wire guide.
Description
Technical Field
The invention relates to the technical field of textile machinery preparation, in particular to Ti 3 SiC 2 A multi-phase composite ceramic wire guide and a preparation method thereof.
Background
Yarn guides, which are one of the important components in modern textile machines, are mainly responsible for the high-speed and stable running of the yarn. The high-speed running of the silk thread often causes great abrasion to the silk guide, and the abrasion resistance of the traditional metal silk guide is poor, so that the use requirement of a modern textile machine cannot be met. Compared with metal materials, the ceramic material has higher hardness and wear resistance, and also has more excellent corrosion resistance, chemical stability and the like, so that ceramic wire guides with excellent comprehensive properties are increasingly applied to the field of textile machinery.
At present, al 2 O 3 And TiO 2 The use of these ceramic wire guides in textile machines is common. However, the above-mentioned ceramic wire guides often exhibit drawbacks such as easy breakage, low wire guide efficiency, short service life, etc. under high-strength working conditions, and the main reasons are that these ceramics themselves have a large friction coefficient, low fracture toughness, low mechanical strength, etc. In view of the foregoing, there is a need to develop a high performance ceramic wire guide with a low coefficient of friction and excellent toughness and strength.
Disclosure of Invention
The inventors of the present invention have made repeated studies on Ti 3 SiC 2 The ceramic is used as a novel ternary carbide material, has the excellent characteristics of ceramic and metal, and is an ideal material for preparing the ceramic wire guide.
Further, the study also found that in Ti 3 SiC 2 Compounding an amount of 3Y-ZrO in a ceramic matrix 2 And B 4 After C, ti can be further enhanced 3 SiC 2 Hardness, wear resistance and fracture toughness of ceramics.
Further, it was found that B powder and C powder were used to generate B in situ during the reaction 4 C, compared with B directly added in the initial powder 4 C has a more excellent effect. And has completed the present invention on the basis of this.
The invention provides a Ti 3 SiC 2 The preparation method of the multi-phase composite ceramic wire guide can prepare the ceramic wire guide with high hardness, high wear resistance and high fracture toughness.
The invention also provides a Ti with high hardness, high wear resistance and high fracture toughness 3 SiC 2 A multi-phase composite ceramic wire guide.
In order to solve the technical problems, the invention adopts the following technical scheme:
ti according to the embodiment of the first aspect of the invention 3 SiC 2 The preparation method of the multi-phase composite ceramic wire guide comprises the following steps:
step S1, ti is mixed with 3 SiC 2 Mixing and dispersing the powder master batch and additive powder to obtain composite powder, wherein the additive powder comprises 3Y-ZrO 2 Powder, B powder and C powder;
s2, mixing the composite powder and an organic binder in a heating mixing internal mixer, crushing the mixed materials, and granulating in a granulator to obtain injection granulating materials;
s3, performing injection molding on the injection granulated material to obtain a composite ceramic wire guide green body;
s4, placing the composite ceramic wire guide blank body into a degreasing furnace for thermal degreasing to obtain a composite ceramic wire guide biscuit;
step S5, heating the composite ceramic biscuit in a vacuum environment, and preserving heat at 1500-1600 ℃ for 30-150min to obtain a sintered body;
step S6, placing the sintered body in a hot isostatic pressing furnace, and performing hot isostatic pressing treatment for 60-180min at 1450-1550 ℃ and 100-150MPa under the inert gas environment to obtain the Ti 3 SiC 2 A multi-phase composite ceramic wire guide.
Further, the content of the additive powder in the composite powder is 20-40wt%,
the 3Y-ZrO 2 The content of the powder in the composite powder is 15-30wt%, and the mol ratio of B to C is (4-5): 1.
further, the Ti is 3 SiC 2 And the powder master batch is nano or submicron powder.
Further, the step S1 includes:
weighing Ti according to a proportion 3 SiC 2 Powder master batch, 3Y-ZrO 2 Powder, powder B and powder C；
Subjecting the Ti to 3 SiC 2 Dispersing the powder master batch and the added powder in alcohol and performing wet ball milling to obtain ball milling slurry;
and (3) carrying out secondary mixing and dispersion on the ball-milling slurry by using a high-power ultrasonic instrument, and drying to obtain the composite powder.
Further, the rotation speed of a ball mill adopted in the wet ball milling is 150-200r/min, and the ball milling time is 16-24h; the secondary mixing is dispersed for 10-20min under the working power of 1500-2000W.
Further, in the step S2,
the organic binder is selected from one or more of polyethylene, polypropylene and paraffin wax, the mixing temperature is 160-200 ℃, the mixing time is 2-4h,
the granulating temperature of the granulating is 160-200 ℃.
Further, in the step S3, the molding temperature is 170-190 ℃ and the injection pressure is 600-800bar during injection molding.
Further, in the step S4, the thermal degreasing temperature is 1000-1200 ℃, and the time and the heat preservation time required for raising the temperature from the room temperature to the degreasing temperature are 60-80 hours in total.
Further, the step S5 includes:
placing the composite ceramic biscuit into a sintering furnace;
vacuumizing the sintering furnace to a vacuum degree of 1-10Pa;
heating the sintering furnace to 1500-1600 ℃ for 4-6h, and preserving heat for 30-150min at 1500-1600 ℃;
and after the heat preservation is finished, cooling along with the furnace.
Ti according to the embodiment of the second aspect of the invention 3 SiC 2 A multi-phase composite ceramic wire guide prepared by the method of any one of the embodiments of the first aspect.
The technical scheme of the invention has at least one of the following beneficial effects:
ti according to an embodiment of the invention 3 SiC 2 Base multiphase composite ceramic conductorPreparation method of silk device by using Ti 3 SiC 2 As a ceramic master batch, ti 3 SiC 2 The graphite structure and the self-lubricating characteristic of the guide wire device lead the guide wire device to have smaller friction coefficient and obvious wear resistance, and the prepared guide wire device has high comprehensive performance and long service life;
at the same time, at Ti 3 SiC 2 Adding 3Y-ZrO into powder 2 Powder, B powder and C powder are used as additive powder, and B is generated in situ in the sintering process 4 C, not only can inhibit the grain growth of other crystal phases and refine the grains, but also can obviously improve the hardness and the wear resistance of the material, can play an excellent role in reinforcing and toughening, and obviously improves Ti 3 SiC 2 The wear resistance and fracture toughness of the ceramic are improved, and the hardness and other properties of the ceramic are improved;
in addition, according to the preparation method of the ceramic wire guide of the embodiment of the invention, firstly, the sintering furnace is vacuumized, and then sintering in a vacuum atmosphere promotes Ti 3 SiC 2 Densification process of the multi-phase composite ceramic wire guide and oxidation prevention of the multi-phase composite ceramic wire guide;
further, the invention uses Ti after vacuum sintering 3 SiC 2 The ceramic wire guide is subjected to Hot Isostatic Pressing (HIP), so that residual air holes in the ceramic are further eliminated, and Ti is improved 3 SiC 2 The compactness of the ceramic wire guide device further improves the hardness, wear resistance and mechanical strength of the material;
ti prepared by the preparation method of the ceramic wire guide according to the embodiment of the invention 3 SiC 2 The multi-phase composite ceramic wire guide has excellent mechanical performance, wear resistance and prolonged service life.
Drawings
FIG. 1 shows the Ti as obtained in example 3 3 SiC 2 A structural schematic diagram of the multi-phase composite ceramic wire guide, wherein (a) is a front view, and (b) is a cross-sectional view;
FIG. 2 is a diagram of Ti obtained in example 3 3 SiC 2 Photographs of the multiple phase composite ceramic wire guide.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which are obtained by a person skilled in the art based on the described embodiments of the invention, fall within the scope of protection of the invention.
Unless defined otherwise, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The terms "first," "second," and the like, as used herein, do not denote any order, quantity, or importance, but rather are used to distinguish one element from another. Likewise, the terms "a" or "an" and the like do not denote a limitation of quantity, but rather denote the presence of at least one. The terms "connected" or "connected," and the like, are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "upper", "lower", "left", "right", etc. are used merely to indicate a relative positional relationship, which changes accordingly when the absolute position of the object to be described changes.
The Ti according to the embodiment of the present invention will be specifically described below 3 SiC 2 A method for preparing a multi-phase composite ceramic wire guide.
Ti according to the embodiment of the first aspect of the invention 3 SiC 2 The preparation method of the multi-phase composite ceramic wire guide comprises the following steps:
step S1, ti is mixed with 3 SiC 2 Mixing and dispersing the powder master batch and additive powder to obtain composite powder, wherein the additive powder comprises 3Y-ZrO 2 Powder, B powder and C powder.
That is, first, ti is used as 3 SiC 2 The powder is used as master batch powder, added with additive powder, and mixed to be used as Ti 3 SiC 2 A raw material of a multi-phase composite ceramic wire guide.
The inventionThrough repeated researches by Ming et al, ti 3 SiC 2 Ti-C in the crystal lattice is in covalent bond combination, the combination bond force is strong, and the performances of high melting point, high modulus and the like of the material are endowed; the bonding force between the Si atoms and Ti-C-Ti-C-Ti chains is weak, and the interlayer weak bonding characteristic is similar to that of graphite with a layered structure. Layered Ti 3 SiC 2 Double layer Ti of ceramics 6 The C octahedra are separated by Si layers and have lamellar properties that are prone to cleavage. Based on this, the layer perpendicular to the C-axis easily slides under the shearing force, so that Ti 3 SiC 2 Has a layered structure and a certain self-lubricity. Ti (Ti) 3 SiC 2 The graphite structure and the self-lubricating property of the wire guide device lead the wire guide device to have smaller friction coefficient and obvious wear resistance, and is suitable for preparing the wire guide device.
In addition, 3Y-ZrO 2 As a structural ceramic with excellent mechanical properties at present, the ceramic has high fracture toughness and high bending strength due to the phase change toughening effect. It was found that an appropriate amount of 3Y-ZrO 2 The introduction as a second phase has a significant effect on the improvement of the fracture toughness of the ceramic matrix. The inventors have also found that, in Ti 3 SiC 2 3Y-ZrO is introduced into the powder master batch 2 The toughness and wear resistance of the final product can be further improved.
B 4 C is used as a light superhard material and has the characteristics of low density, high elastic modulus, corrosion resistance, abrasion resistance and the like. It was found that the proper amount of B was incorporated into the ceramic matrix 4 After C, the crystal grain growth of other crystal phases can be inhibited, the crystal grains are refined, and the hardness and the wear resistance of the material are obviously improved. However, if B is added directly to the initial powder 4 The C powder has larger difference with the base metal due to the hardness and thermal expansion coefficient, so that the C powder is easy to crack and the like. The inventors found through a large number of experiments that Ti 3 SiC 2 Sintering conditions of the ceramics are favorable for B 4 In situ synthesis of C, B produced under such conditions 4 C has a fine microstructure and can play a role in enhancing and toughening. Thus, by adding Ti to 3 SiC 2 B powder and C powder are introduced into the powder master batch, and B powder is generated in situ in the sintering process 4 C has good effect on improving the hardness and mechanical strength of the ceramic.
In some embodiments of the present invention, the additive powder is present in the composite powder in an amount of 20 to 40wt%, the 3Y-ZrO 2 The content of the powder in the composite powder is 15-30wt%, and the mol ratio of B to C is (4-5): 1.
that is, ti of the embodiment of the invention 3 SiC 2 Multi-phase ceramic composite powder material is prepared from Ti 3 SiC 2 The powder master batch is added with additive powder with the total content of 20-40wt%, wherein 3Y-ZrO 2 15-30wt% of powder, and the balance of B and C.
It has been found that the addition of the additive powder in the above ratio range increases Ti to some extent 3 SiC 2 Mechanical properties such as wear resistance, fracture toughness, bending strength and the like of the multi-phase composite ceramic wire guide. The addition content is too low, and the improvement of the comprehensive performance can not reach the expected effect; if the content of the additive is too high, ti is caused 3 SiC 2 Ceramic sintering densification is difficult, comprehensive performance is reduced, and production cost is increased.
In addition, the inventors have found that B undergoes a slight doping into Ti during sintering 3 SiC 2 In the crystal lattice, this doping is advantageous for further refinement of the grains. Accordingly, to compensate for this portion of doping, compared to B 4 The chemical equivalent of B and C in C (molar ratio of 4:1, mass ratio of about 3.6:1) is added with a little higher than the chemical equivalent of B, for example, the molar ratio is (4-5): 1, so that the doping effect of B can be utilized and the doping effect of B can be simultaneously considered 4 In situ synthesis of C. Preferably, the mass ratio of the mass B to the mass C is 4:1.
In some embodiments of the invention, the Ti 3 SiC 2 And the powder master batch is nano or submicron powder.
The size range of the additive powder selected in the experiment is based on the comprehensive consideration of the performance and the production cost. The above-mentioned size range of the additive powder not only has stable performance, but also has been found to contribute to the improvement of sinterability by using nano-or submicron powderCan improve the density, is favorable for the uniform dispersion of the powder and synthesizes the B in situ 4 C can be uniformly dispersed in the ceramic matrix, is favorable for refining grains and has good material comprehensive performance. In addition, the raw materials in the size range are wide in source and low in cost, can be purchased from a plurality of ceramic powder raw material enterprises and reagent platforms in China, and have high comprehensive cost performance.
Further, the step S1 includes:
weighing Ti according to a proportion 3 SiC 2 Powder master batch, 3Y-ZrO 2 Powder, B powder and C powder;
subjecting the Ti to 3 SiC 2 Dispersing the powder master batch and the added powder in alcohol and performing wet ball milling to obtain ball milling slurry;
and (3) carrying out secondary mixing and dispersion on the ball-milling slurry by using a high-power ultrasonic instrument, and drying to obtain the composite powder.
Through secondary mixing and dispersing, better dispersing effect can be achieved. That is, ti is weighed according to the above ratio 3 SiC 2 The powder and various functional powders are subjected to wet ball milling to obtain uniformly mixed slurry, and agglomerated particles are further removed through secondary mixing and dispersion, so that the composite powder which is fully and uniformly dispersed and basically consistent in granularity is finally obtained.
In some embodiments of the invention, the rotational speed of the ball mill adopted in the wet ball milling is 150-200r/min, and the ball milling time is 16-24h; the secondary mixing is dispersed for 10-20min under the working power of 1500-2000W.
The process is beneficial to improving uniformity, and can obtain the mixed powder which is sufficiently dried and is not easy to agglomerate.
And S2, mixing the composite powder and the organic binder in a heating mixing internal mixer, crushing the mixed materials, and granulating in a granulator to obtain injection granulating materials.
That is, after the composite powder is obtained, the injection pellets can be obtained by kneading with an organic binder under heating and granulating.
In some embodiments of the present invention, the organic binder is selected from one or more of Polyethylene (PE), polypropylene (PP) and paraffin wax, the mixing temperature is 160-200 ℃, the mixing time is 2-4 hours, and the granulating temperature of the granulating is 160-200 ℃.
And step S3, performing injection molding on the injection granulated material to obtain a composite ceramic wire guide green body.
And (3) performing injection molding by using an injection molding machine to obtain the injection molding granules after granulation, so as to obtain the composite ceramic wire guide green body.
In some embodiments of the present invention, in the step S3, the injection molding temperature is 170-190 ℃ and the injection pressure is 600-800bar.
And S4, placing the composite ceramic wire guide blank body into a degreasing furnace for thermal degreasing to obtain the composite ceramic wire guide biscuit.
In the step S4, the thermal degreasing temperature is 1000-1200 ℃, and the total time and the heat preservation time required for raising the temperature from the room temperature to the degreasing temperature are 60-80 hours. (degreasing is a longer process, the temperature rise and reduction speed is low, and the thermal insulation degreasing time is long)
The organic binder used for granulation can be removed by degreasing. In order to avoid collapse of the green body, etc. caused by too high a temperature rising speed, the degreasing process preferably uses a slow temperature rising speed, for example, the degreasing process can slowly raise the temperature to 1000-1200 ℃ over 48-60 h.
And S5, heating the composite ceramic biscuit in a vacuum environment, and preserving heat at 1500-1600 ℃ for 30-150min to obtain a sintered body.
The degreased composite ceramic biscuit can be sintered for one time in a vacuum environment.
In some embodiments of the present invention, the step S5 specifically includes:
placing the composite ceramic biscuit into a sintering furnace;
vacuumizing the sintering furnace to a vacuum degree of 1-10Pa;
heating the sintering furnace to 1500-1600 ℃ for 4-6h, and preserving heat for 30-150min at 1500-1600 ℃;
and after the heat preservation is finished, cooling along with the furnace.
Firstly, the sintering furnace is vacuumized, and then sintered in vacuum atmosphere, so that Ti is promoted 3 SiC 2 Densification process of the multi-phase composite ceramic wire guide, prevents B and C from being oxidized in sintering process, and promotes in-situ synthesis of B under reaction conditions 4 C。
Step S6, placing the sintered body in a hot isostatic pressing furnace, and performing hot isostatic pressing treatment for 60-180min at 1450-1550 ℃ and 100-150MPa under the inert gas environment to obtain the Ti 3 SiC 2 A multi-phase composite ceramic wire guide.
That is, after vacuum sintering, further Hot Isostatic Pressing (HIP) treatment is performed under hot isostatic pressing conditions. The further Hot Isostatic Pressing (HIP) treatment is beneficial to further eliminating the pores in the ceramic and improving the compactness and the material performance.
As the inert gas, for example, argon or the like which is different from Ti can be used 3 SiC 2 And (3) generating a gas for reacting the multiphase composite ceramic.
In addition, after the hot isostatic pressing treatment, the method may further comprise the following steps according to the appearance requirement, the use requirement and the like of the product:
step S7, for the Ti obtained in the step S6 3 SiC 2 Vibration polishing treatment is carried out on the multi-phase composite ceramic wire guider to obtain Ti with smooth and compact surface 3 SiC 2 And (5) a multi-phase composite ceramic wire guide end product.
Ti prepared by the preparation method of the ceramic wire guide according to the embodiment of the invention 3 SiC 2 The multi-phase composite ceramic wire guide has excellent mechanical performance and long service life.
The Ti of the present invention will be described in further detail by the following specific examples 3 SiC 2 Preparation method of multi-phase composite ceramic wire guide and Ti obtained by same 3 SiC 2 A multi-phase composite ceramic wire guide.
Example 1
(1) Raw materials
Respectively weigh 8.0kg of Ti 3 SiC 2 Powder master batch (Ti) 3 SiC 2 Particle size 0.4 μm, available from Fosman technology (Beijing); and (3) adding powder: 1.5kg of 3Y-ZrO 2 Powder, 0.1kg of C powder and 0.4kg of B powder.
Wherein 3Y-ZrO 2 The particle size is 0.15 mu m, the particle size of the powder B is 0.2 mu m, the particle size of the powder C is 0.5 mu m, and the raw materials are purchased from Chinese medicine groups.
(2) Preparation of ceramic wire guide
Dispersing the ceramic powder in alcohol, and performing wet ball milling by adopting a ball mill, wherein the ball milling rotating speed is 180r/min, and the ball milling time is 20h.
And (3) performing secondary mixing dispersion on the slurry after ball milling by using a high-power ultrasonic instrument, and performing ultrasonic dispersion for 15min under the power of 2000W.
The powder slurry after ultrasonic dispersion is dried and sieved, and then is evenly mixed with organic binders such as Polyethylene (PE), polypropylene (PP), paraffin and the like under the heating condition, and mixed for 3 hours at the temperature of 180 ℃.
Granulating the mixed powder by using a granulator at a granulating temperature of 180 ℃ to obtain injection granulating materials.
And (3) performing injection molding on the injection granulated material by using an injection machine, wherein the molding temperature is 180 ℃, and the pressure is 700bar, so as to obtain a composite ceramic wire guide green body containing the organic binder.
And (3) performing thermal degreasing treatment on the composite ceramic wire guide blank body to remove more organic binders in the ceramic blank body, wherein the degreasing temperature is 1100 ℃, and the total time and the heat preservation time required for raising the degreasing temperature from the room temperature are 70h.
Will be free of binder Ti 3 SiC 2 And (5) carrying out vacuum sintering on the composite ceramic biscuit. Specifically, the furnace is first vacuumized to a vacuum degree of 5Pa, then heated to 1550 ℃ for 5 hours, kept at the temperature for 90 minutes and then cooled with the furnace. Subjecting the vacuum sintered sample to Hot Isostatic Pressing (HIP) at 1500deg.C for 120min, the furnace gas pressure was maintained at 125MPa.
Finally, placing the composite ceramic wire guide subjected to Hot Isostatic Pressing (HIP) treatment into a vibration polishing machine, wherein polishing media in the polishing machine are diamond and water, performing vibration polishing for 30 hours, and performing ultrasonic cleaning and drying on the polished ceramic wire guide to obtain Ti 3 SiC 2 And (5) a multi-phase composite ceramic wire guide end product.
Example 2
(1) Raw materials
Respectively weigh 7.0kg Ti 3 SiC 2 Powder master batch (Ti) 3 SiC 2 Particle size 0.4 μm, available from Fosman technology (Beijing); and (3) adding powder: 2.0kg of 3Y-ZrO 2 Powder, 0.2kg of C powder and 0.8kg of B powder (3Y-ZrO 3 2 The particle size is 0.15 μm, the particle size of the powder B is 0.2 μm, the particle size of the powder C is 0.5 μm, and the raw materials are all purchased from Chinese medicine group).
(2) Preparation of ceramic wire guide
A ceramic wire guide was prepared in the same manner as in example 1 above, except that the raw material content was different from example 1 above.
Example 3
(1) Raw materials
Weighing 6.0kg of Ti 3 SiC 2 Powder master batch (Ti) 3 SiC 2 Particle size 0.4 μm, available from Fosman technology (Beijing); and (3) adding powder: 2.5kg of 3Y-ZrO 2 Powder, 0.3kg of C powder and 1.2kg of B powder (3Y-ZrO 3 2 The particle size is 0.15 μm, the particle size of the powder B is 0.2 μm, the particle size of the powder C is 0.5 μm, and the raw materials are all purchased from Chinese medicine group).
(2) Preparation of ceramic wire guide
A ceramic wire guide was prepared in the same manner as in example 1 above, except that the raw material content was different from example 1 above.
Fig. 1 shows a schematic structural view of a ceramic wire guide, and fig. 2 shows a ceramic wire guide finished product finally obtained by polishing.
As can be seen from fig. 1 and 2, the ceramic guide wire prepared has a very high surface gloss, which further indicates that the compactness is relatively high.
Example 4
(1) Raw materials
Weighing 5.0kg of Ti respectively 3 SiC 2 Powder master batch (Ti) 3 SiC 2 Particle size 0.4 μm, available from Fosman technology (Beijing); and (3) adding powder: 3.0kg of 3Y-ZrO 2 Powder, 0.4kg of C powder and 1.6kg of B powder (3Y-ZrO 3 2 The particle size is 0.15 μm, the particle size of the powder B is 0.2 μm, the particle size of the powder C is 0.5 μm, and the raw materials are all purchased from Chinese medicine group).
(2) Preparation of ceramic wire guide
A ceramic wire guide was prepared in the same manner as in example 1 above, except that the raw material content was different from example 1 above.
Example 5
The content of each raw material was the same as in example 3.
The only difference from example 3 is that: the granulation temperature during granulation was 200 ℃.
Example 6
The content of each raw material was the same as in example 3.
The only difference from example 3 is that: the degreasing temperature in the thermal degreasing process is 1000 ℃.
Example 7
The content of each raw material was the same as in example 3.
The only difference from example 3 is that: the degreasing temperature in the thermal degreasing process is 1200 ℃.
Example 8
The content of each raw material was the same as in example 3.
The only difference from example 3 is that: the temperature during the vacuum sintering process was 1500 ℃.
Example 9
The content of each raw material was the same as in example 3.
The only difference from example 3 is that: the temperature during vacuum sintering was 1600 ℃.
Comparative example 1
Weigh 10.0kg of Ti 3 SiC 2 Powder master batch (Ti) 3 SiC 2 The particle size was 0.4 μm, purchased from Fosman technology (Beijing) Co., ltd.), and did not contain any additive powder.
And a ceramic wire guide was prepared by the same preparation method as in example 1.
Comparative example 2
Weigh 7.0kg of Ti 3 SiC 2 Powder master batch (Ti) 3 SiC 2 Particle size 0.4 μm, available from Fosman technology (Beijing); and (3) adding powder: 3.0kg of 3Y-ZrO 2 (3Y-ZrO 2 The particle size is 0.15 μm, and the raw materials are purchased from China medicine group).
And a ceramic wire guide was prepared by the same preparation method as in example 1.
Comparative example 3
Weigh 7.0kg Ti 3 SiC 2 Powder master batch (Ti) 3 SiC 2 Particle size 0.4 μm, available from Fosman technology (Beijing); and (3) adding powder: 0.5kg of B powder and 2.5kg of C powder (the particle size of the B powder is 0.2 mu m, the particle size of the C powder is 0.5 mu m, and the raw materials are all purchased from Chinese medicine group).
And a ceramic wire guide was prepared by the same preparation method as in example 1.
Comparative example 4
The content of each raw material was the same as in example 3.
The only difference from example 3 is that: the vacuum sintered sample is not subjected to Hot Isostatic Pressing (HIP), but is directly polished to obtain a ceramic wire guide finished product.
Comparative example 5
Weigh 7.0kg Ti 3 SiC 2 Powder master batch (Ti) 3 SiC 2 Particle size 0.4 μm, available from Fosman technology (Beijing); and (3) adding powder: 3.0kg B 4 C(B 4 C has a particle size of 0.2 μm and is obtained from China medicine group).
And a ceramic wire guide was prepared by the same preparation method as in example 1.
The ceramic wire guides prepared in the above examples and comparative examples 1 to 5 were tested to obtain the average properties shown in table 1 below.
Table 1 average performance test results for each of examples and comparative examples
As is clear from the above table, the Ti of the present invention 3 SiC 2 Ceramic powder used by multi-phase composite ceramic wire guider is prepared from Ti 3 SiC 2 Adding proper amount of 3Y-ZrO powder into the powder 2 Powder, B powder and C powder, by vacuum sintering and Hot Isostatic Pressing (HIP) treatment after sintering, ti is overcome 3 SiC 2 The ceramic has the defects of low sintering compactness, poor toughness, low mechanical strength and the like, so that the service performance of the product is greatly improved, and the service life of the product is prolonged.
In contrast, the comparative examples were prepared by adding no additional powder of the present invention or only a part of the additional powder and directly adding B to the initial powder 4 The combination property of the comparative examples of the powder C is far lower than that of the test results of the examples of the invention.
Furthermore, from the above test results, it is clear that example 3 of the present invention is particularly remarkable in terms of the formulation composition and the properties obtained under the process conditions.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (9)
1. Ti (titanium) 3 SiC 2 The preparation method of the multi-phase composite ceramic wire guide is characterized by comprising the following steps:
step S1, ti is mixed with 3 SiC 2 Mixing and dispersing the powder master batch and additive powder to obtain composite powder, wherein the additive powder is prepared from 3Y-ZrO 2 Powder, B powder and C powder, wherein the content of the additive powder in the composite powder is 20-40wt%, and the content of the 3Y-ZrO is as follows 2 The content of the powder in the composite powder is 15-30wt%The mol ratio of the powder B to the powder C is (4-5): 1, a step of;
s2, mixing the composite powder and an organic binder in a heating mixing internal mixer, crushing the mixed materials, and granulating in a granulator to obtain injection granulating materials;
s3, performing injection molding on the injection granulated material to obtain a composite ceramic wire guide green body;
s4, placing the composite ceramic wire guide blank body into a degreasing furnace for thermal degreasing to obtain a composite ceramic wire guide biscuit;
step S5, heating the composite ceramic wire guide biscuit in a vacuum environment, and preserving heat at 1500-1600 ℃ for 30-150min to obtain a sintered body;
step S6, placing the sintered body in a hot isostatic pressing furnace, and performing hot isostatic pressing treatment for 60-180min at 1450-1550 ℃ and 100-150MPa under the inert gas environment to obtain the Ti 3 SiC 2 A multi-phase composite ceramic wire guide.
2. Ti according to claim 1 3 SiC 2 The preparation method of the multi-phase composite ceramic wire guide is characterized by comprising the following steps of 3 SiC 2 And the powder master batch is nano or submicron powder.
3. Ti according to claim 1 3 SiC 2 The preparation method of the multi-phase composite ceramic wire guide is characterized in that the step S1 comprises the following steps:
weighing Ti according to a proportion 3 SiC 2 Powder master batch, 3Y-ZrO 2 Powder, B powder and C powder;
subjecting the Ti to 3 SiC 2 Dispersing the powder master batch and the added powder in alcohol and performing wet ball milling to obtain ball milling slurry;
and (3) carrying out secondary mixing and dispersion on the ball-milling slurry by using a high-power ultrasonic instrument, and drying to obtain the composite powder.
4. A Ti according to claim 3 3 SiC 2 The preparation method of the multi-phase composite ceramic wire guide is characterized in that the rotation speed of a ball mill adopted in wet ball milling is 150-200r/min, and the ball milling time is 16-24h; the secondary mixing is dispersed for 10-20min under the working power of 1500-2000W.
5. Ti according to claim 1 3 SiC 2 The preparation method of the multi-phase composite ceramic wire guide is characterized in that in the step S2,
the organic binder is selected from one or more of polyethylene, polypropylene and paraffin wax, the mixing temperature is 160-200 ℃, the mixing time is 2-4h,
the granulating temperature of the granulating is 160-200 ℃.
6. Ti according to claim 1 3 SiC 2 The preparation method of the multi-phase composite ceramic wire guide is characterized in that in the step S3, the molding temperature is 170-190 ℃ and the injection pressure is 600-800bar during injection molding.
7. The method according to claim 1, wherein in the step S4, the thermal degreasing temperature is 1000-1200 ℃, and the total time required for raising the temperature from the room temperature to the degreasing temperature and the holding time are 60-80h.
8. Ti according to claim 1 3 SiC 2 The preparation method of the multi-phase composite ceramic wire guide is characterized in that the step S5 comprises the following steps:
placing the composite ceramic wire guide biscuit into a sintering furnace;
vacuumizing the sintering furnace to a vacuum degree of 1-10Pa;
heating the sintering furnace to 1500-1600 ℃ for 4-6h, and preserving heat for 30-150min at 1500-1600 ℃;
and after the heat preservation is finished, cooling along with the furnace.
9. Ti (titanium) 3 SiC 2 A multiphase composite ceramic wire guide, characterized in that it is made of Ti according to any one of claims 1 to 8 3 SiC 2 The preparation method of the multi-phase composite ceramic wire guide is used for preparing the multi-phase composite ceramic wire guide.
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