CN109940162B - Preparation method of titanium carbide in-situ reinforced titanium and titanium alloy stent - Google Patents
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Abstract
The invention discloses a preparation method of a porous support of carbide in-situ reinforced titanium and alloy thereof. According to the invention, the distribution of sucrose and graphene in the hole wall is controlled by utilizing a freeze drying technology, the sucrose on the inner wall of the hole and the graphene in the hole wall react with titanium in situ to generate enhanced phase titanium carbide in the vacuum sintering process, and the generation amount of the titanium carbide in the hole wall is controlled by regulating the addition amount of the sucrose and the graphene, so that the impact-resistant titanium and the alloy bracket thereof with high strength, good combination of a matrix and a second phase interface are obtained, and the titanium and the alloy bracket thereof have wide application prospects in the fields of aerospace, automobile manufacturing, biomedicine and the like.
Description
Technical Field
The invention belongs to the technical field of material preparation, and relates to a preparation method of a titanium carbide in-situ reinforced titanium and titanium alloy bracket.
Background
With the advance of the wave of new technology revolution, the traditional titanium and titanium alloy have been increasingly difficult to meet the high technology requirement. Titanium-based composites refer to a composite that incorporates reinforcement into the titanium or titanium alloy. The titanium alloy has ductility and toughness of a matrix and high strength and modulus of a reinforcement, so that the titanium alloy has higher specific strength, specific rigidity and high temperature resistance than titanium or titanium alloy, and has excellent designability, and therefore, the titanium alloy has increasingly received attention of researchers at home and abroad in recent years.
The particle reinforced titanium-based composite material has excellent performances of high specific strength, high elastic modulus, good wear resistance, high-temperature creep resistance and the like, so that the particle reinforced titanium-based composite material is widely applied to the fields of aerospace, automobile manufacturing, biomedicine and the like. The titanium carbide has small thermal expansion coefficient, high hardness, good thermal stability and low friction coefficient, and has density similar to that of titanium alloy and can be used as a titanium-based composite material reinforcement. Aiming at the problem of low bonding strength of a microscopic interface, the in-situ reaction method is a feasible method for improving the bonding strength of the reinforcement/matrix interface. Therefore, the titanium carbide particles generated by the in-situ reaction have important significance in enhancing the strength and rigidity of the titanium alloy bracket.
A patent of a low-cost industrial production method of TiC particle reinforced titanium-based composite material (application No. 201711437226.8, published as 2018-06-22, publication No. 108193064A discloses a low-cost industrial production method of TiC particle reinforced titanium-based composite material, which integrates a process of producing titanium powder by hydrogenation and dehydrogenation and a process of adding a composite material reinforcing phase to integrally produce the TiC particle reinforced titanium-based composite material, and the prepared material reinforcing phase is uniformly distributed and has a certain effect of improving the strength, but the rigidity is insufficient and the impact resistance is insufficient.
A patent of a preparation method of TiB enhanced medical porous titanium (application number: 201811528721.4, published: 2019-02-15, published: 109332700A discloses a preparation method of TiB enhanced medical porous titanium, which comprises the steps of firstly, Ti powder and TiB2Powder and pore-forming agent NH4HCO3Weighing according to a certain proportion, then uniformly mixing under the protection of argon, then carrying out vacuum sintering by using a discharge plasma sintering furnace, and finally carrying out vacuum heat treatment to obtain the TiB reinforced medical porous titanium with low elastic modulus, high strength and moderate porosity, wherein the reinforcing phase TiB is unevenly distributed in a matrix.
The patent application No. 201410372169.X, published as: 2015-12-09, and publication No. 104141063B discloses a preparation method of an in-situ synthesized titanium carbide reinforced titanium-based porous material, which adopts a powder metallurgy pore-forming agent technology, uses urea, carbon powder and titanium powder to prepare a porous titanium-based composite material with high strength and good corrosion resistance through the steps of mixing, pressing and sintering, but the impact resistance of the porous titanium-based composite material is insufficient.
In the document "Particulate reinforced titanium alloy compositions formed by combining particles and hot isostatic pressing" (1993, Industral heating, volume 60, pages 32-37), TiC and other reinforcing particles are artificially added into a titanium alloy by a composite method and are prepared by an external addition method, but the method cannot fundamentally solve the problems of uniform distribution of a reinforcement, complete combination of the reinforcement and a matrix and the like, and the pollution of the reinforcement can reduce the performance of the material.
Disclosure of Invention
The invention aims to provide a preparation method of a titanium carbide in-situ reinforced titanium and titanium alloy stent, which solves the problems of poor interface bonding, low strength and insufficient impact resistance of a titanium and titanium alloy porous stent reinforcement and a matrix in the prior art.
The technical scheme adopted by the invention is that the preparation method of the titanium carbide in-situ reinforced titanium and titanium alloy bracket comprises the steps of adding cane sugar and graphene into a suspension containing a titanium source, uniformly mixing, injecting into a mold, and carrying out freeze drying and vacuum sintering to obtain the titanium carbide in-situ reinforced titanium and titanium alloy bracket.
The method is implemented by the following steps:
step 1, sequentially adding a dispersing agent, a binder and titanium source powder into a solvent, and uniformly mixing for 20-24 hours to obtain a suspension;
step 2, adding cane sugar into the turbid liquid obtained in the step 1, uniformly stirring, adding graphene, and performing ball milling for 12-24 hours to obtain composite slurry;
step 3, injecting the composite slurry obtained in the step 2 into a mold, performing directional freezing on a cold source, taking out the suspension after the suspension is completely frozen, and drying in a low-pressure environment to obtain a support preform;
and 4, sintering the support preform obtained in the step 3 at high temperature in vacuum to obtain the titanium carbide in-situ reinforced titanium and titanium alloy support.
In the step 1, the solvent is distilled water or a mixed solution of distilled water and tert-butyl alcohol, the titanium source powder is one of titanium hydride, pure titanium or titanium alloy, the dispersing agent is one of sodium polyacrylate, sodium methylene dinaphthalene sulfonate, sodium dodecyl benzene sulfonate or polyvinylpyrrolidone, and the binder is one of polyvinyl alcohol, hydroxymethyl cellulose, citric acid or polyvinyl butyral.
In the step 1, the volume ratio of the titanium source powder to the solvent is 1: 2-5, the mass of the dispersing agent accounts for 0.5-2% of the mass of the titanium source powder, and the mass of the binder accounts for 0.2-3% of the mass of the titanium source powder.
In the step 2, the mass of the sucrose accounts for 5-20% of the mass of the titanium source powder, and the mass of the graphene accounts for 0.5-4% of the mass of the titanium source powder.
In the step 3, the freezing temperature is-120 ℃ to-30 ℃ during directional freezing, the cooling rate is 5-15 mu m/s, and the freezing time is 1.5-3 h.
In step 3, the bottom of the mold is made of heat conducting material, and the heat conducting material is aluminum, copper or silver.
In the step 3, the pressure of the low-pressure environment is 10-100 Pa.
In the step 4, the sintering temperature is 1200-1400 ℃, and the sintering time is 1.5-3 h.
The method has the beneficial effects that the freeze drying technology is utilized, the distribution of the sucrose and the graphene in the hole wall is controlled, and the reinforced phase titanium carbide is generated through in-situ reaction during sintering, so that the impact-resistant titanium and titanium alloy bracket with high strength, good combination of a matrix and a second phase interface is obtained, and the method has wide application prospects in the fields of aerospace, automobile manufacturing, biomedicine and the like.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a preparation method of a titanium carbide in-situ reinforced titanium and titanium alloy bracket.
The method is implemented by the following steps:
step 1, sequentially adding a dispersing agent, a binder and titanium source powder into a solvent, and uniformly mixing for 20-24 hours to obtain a suspension;
step 2, adding cane sugar into the turbid liquid obtained in the step 1, uniformly stirring, adding graphene, and performing ball milling for 12-24 hours to obtain composite slurry;
step 3, injecting the composite slurry obtained in the step 2 into a mold, performing directional freezing on a cold source, taking out the suspension after the suspension is completely frozen, and drying in a low-pressure environment to obtain a support preform;
and 4, sintering the support preform obtained in the step 3 at high temperature in vacuum to obtain the titanium carbide in-situ reinforced titanium and titanium alloy support.
In the step 1, the solvent is distilled water or a mixed solution of distilled water and tert-butyl alcohol, the titanium source powder is one of titanium hydride, pure titanium or titanium alloy, the dispersing agent is one of sodium polyacrylate, sodium methylene dinaphthalene sulfonate, sodium dodecyl benzene sulfonate or polyvinylpyrrolidone, and the binder is one of polyvinyl alcohol, hydroxymethyl cellulose, citric acid or polyvinyl butyral.
In the step 1, the volume ratio of the titanium source powder to the solvent is 1: 2-5, the mass of the dispersing agent accounts for 0.5-2% of the mass of the titanium source powder, and the mass of the binder accounts for 0.2-3% of the mass of the titanium source powder.
In the step 2, the mass of the sucrose accounts for 5-20% of the mass of the titanium source powder, and the mass of the graphene accounts for 0.5-4% of the mass of the titanium source powder.
In the step 3, the freezing temperature is-120 ℃ to-30 ℃ during directional freezing, the cooling rate is 5-15 mu m/s, and the freezing time is 1.5-3 h.
In step 3, the bottom of the mold is made of heat conducting material, and the heat conducting material is aluminum, copper or silver.
In the step 3, the pressure of the low-pressure environment is 10-100 Pa.
In the step 4, the sintering temperature is 1200-1400 ℃, and the sintering time is 1.5-3 h.
The matrix in the invention is a porous support of titanium and titanium alloy, and titanium, graphene and cane sugar are subjected to in-situ reaction to generate titanium carbide in-situ reinforced titanium and titanium alloy supports.
The invention relates to a preparation method of a titanium carbide in-situ reinforced titanium and titanium alloy bracket, which is characterized in that sucrose and graphene are added into a solution, the mixture is subjected to ball milling to obtain a composite slurry, a directional freeze drying technology is utilized, the concentration of sucrose at the tip of an ice crystal is increased in the freezing process, the sucrose is pushed to two sides of the ice crystal and is mainly distributed on the inner wall of a hole, a titanium carbide layer with a certain thickness is formed in situ on the inner wall of the titanium and the titanium alloy hole after high-temperature vacuum sintering, and the titanium carbide layer has higher rigidity relative to the bracket, so that the deformation resistance of the porous bracket is increased when the porous bracket is subjected to impact load, and a large amount of energy is consumed by.
In addition, the added graphene is uniformly dispersed in the slurry, and the graphene is uniformly dispersed in the porous pore walls after directional freezing. And after vacuum sintering, reacting the graphene with titanium to generate titanium carbide. The interface bonding property of the titanium carbide reinforcement obtained by the in-situ reaction and the matrix is good, when bearing load, the titanium carbide particles can block the crack from expanding or deflect, the crack path is tortuous, more fracture energy is consumed, and the strength of the material is improved.
Example 1
0.348g of sodium polyacrylate, 0.696g of carboxymethyl cellulose and 34.8g of TiH were added to 50g of distilled water in this order2Powder, TiH2The mass ratio of the powder to the distilled water is 1:5, the mixture is fully mixed for 20 hours, then 1.74g of cane sugar and 0.696g of graphene are added, ball milling is carried out for 20 hours to obtain slurry, and TiH is added2Injecting the slurry into a cylindrical mold with a side wall made of polyethylene and a bottom made of heat conducting materials, directionally freezing for 3 hours at the temperature of-30 ℃ on an ethanol liquid cold source with the cooling rate of 15 mu m/s, completely freezing, then placing in the environment of 10pa for low-pressure drying to obtain a blank of the support, and sintering in vacuum at the temperature of 1300 ℃ for 1.5 hours to obtain the titanium carbide in-situ reinforced titanium and titanium alloy support.
Example 2
Adding 1.804g of sodium dodecyl benzene sulfonate, 0.1804g of polyvinyl alcohol and 90.2g of pure Ti powder into 40g of distilled water in sequence, wherein the mass ratio of the pure Ti powder to the distilled water is 1:2, fully mixing for 22h, then adding 9.02g of sucrose and 0.451g of graphene, ball-milling for 24h to obtain slurry, injecting the Ti slurry into a cylindrical mold with a side wall made of polyethylene and a bottom made of heat conducting material, directionally freezing for 1.5h on a methanol liquid cold source at minus 60 ℃, cooling at the rate of 10 mu m/s, completely freezing, drying in a 40pa environment at low pressure to obtain a support blank, sintering at 1200 ℃ in vacuum, and sintering for 2h to obtain the titanium carbide in-situ reinforced titanium and titanium alloy supports.
Example 3
To a 50g of a distilled water/t-butanol mixed solution were added 1.414g of polyvinylpyrrolidone, 0.707g of polyvinyl butyral, and 70.7g of Ti in this order6Al4V powder, Ti6Al4The mass ratio of the V powder to the distilled water/tert-butyl alcohol is 1:4, after fully mixing for 24 hours, 9.191g of sucrose and 2.121g of graphene are added, ball milling is carried out for 22 hours to obtain slurry, and Ti is added6Al4Injecting the V slurry into a cylindrical mold with a side wall made of polyethylene and a bottom made of a heat conducting material, directionally freezing for 2 hours at the temperature of minus 90 ℃ by using a mixed liquid cold source of liquid nitrogen and ethanol, wherein the cooling rate is 5 mu m/s, completely freezing, drying in an environment of 20pa at low pressure to obtain a support blank, sintering in vacuum at 1200 ℃, and sintering for 2.5 hours to obtain the titanium carbide in-situ reinforced titanium and titanium alloy support.
Example 4
0.2825g of polyvinylpyrrolidone, 1.695g of citric acid and 56.5g of pure Ti powder are sequentially added into 30g of distilled water/tert-butyl alcohol mixed solution, the mass ratio of the pure Ti powder to the distilled water/tert-butyl alcohol is 1:3, after the pure Ti powder and the distilled water/tert-butyl alcohol are fully mixed for 23 hours, 11.3g of cane sugar and 2.26g of graphene are added, the mixture is ball-milled for 12 hours to obtain slurry, and Ti is mixed with the slurry6Al4Injecting the V slurry into a cylindrical mold with a side wall made of polyethylene and a bottom made of a heat conducting material, directionally freezing for 3 hours at the temperature of minus 120 ℃ by using a mixed liquid cold source of liquid nitrogen and methanol, wherein the cooling rate is 15 mu m/s, completely freezing, placing in an environment of 100pa, drying at low pressure to obtain a blank of the support, sintering at the temperature of 1400 ℃ in vacuum, and sintering for 3 hours to obtain the titanium carbide in-situ reinforced titanium and titanium alloy support.
Table 1 shows the porosity and compressive strength of the titanium carbide in-situ reinforced titanium and titanium alloy scaffolds prepared in examples 1, 2, 3 and 4 of the present invention as shown in table 1:
TABLE 1 porosity and compressive strength of in-situ reinforced titanium
The table shows that the compressive property of the porous scaffold is remarkably improved by adding carbon source sucrose to react with graphene in situ to generate the enhanced phase titanium carbide, and the porosity is slightly increased along with the increase of the sucrose content.
According to the invention, the freeze drying technology is utilized to control the distribution of sucrose and graphene in the hole wall, and the enhanced phase titanium carbide is generated through in-situ reaction during sintering, so that the impact-resistant titanium and titanium alloy support with high strength, good combination of a matrix and a second phase interface is obtained, and the titanium and titanium alloy support has a wide application prospect in the fields of aerospace, automobile manufacturing, biomedicine and the like.
Claims (8)
1. A preparation method of a titanium carbide in-situ reinforced titanium and titanium alloy bracket is characterized in that cane sugar and graphene are added into a suspension containing a titanium source, the mixture is uniformly mixed and then injected into a mold, and the mold is freeze-dried and vacuum-sintered to obtain the titanium carbide in-situ reinforced titanium and titanium alloy bracket;
the method is implemented by the following steps:
step 1, sequentially adding a dispersing agent, a binder and titanium source powder into a solvent, and uniformly mixing for 20-24 hours to obtain a suspension;
step 2, adding cane sugar into the turbid liquid obtained in the step 1, uniformly stirring, adding graphene, and performing ball milling for 12-24 hours to obtain composite slurry;
step 3, injecting the composite slurry obtained in the step 2 into a mold, performing directional freezing on a cold source, taking out the suspension after the suspension is completely frozen, and drying in a low-pressure environment to obtain a support preform;
and 4, sintering the support preform obtained in the step 3 at high temperature in vacuum to obtain the titanium carbide in-situ reinforced titanium and titanium alloy support.
2. The method for preparing the titanium carbide in-situ reinforced titanium and titanium alloy stent as claimed in claim 1, wherein in the step 1, the solvent is distilled water or a mixed solution of distilled water and t-butyl alcohol, the titanium source powder is one of titanium hydride, pure titanium or titanium alloy, the dispersing agent is one of sodium polyacrylate, sodium methylene dinaphthalene sulfonate, sodium dodecyl benzene sulfonate or polyvinylpyrrolidone, and the binder is one of polyvinyl alcohol, hydroxymethyl cellulose, citric acid or polyvinyl butyral.
3. The method for preparing the titanium carbide in-situ reinforced titanium and titanium alloy stent according to claim 1, wherein in the step 1, the volume ratio of the titanium source powder to the solvent is 1: 2-5, the mass of the dispersing agent accounts for 0.5-2% of the mass of the titanium source powder, and the mass of the bonding agent accounts for 0.2-3% of the mass of the titanium source powder.
4. The method for preparing the titanium carbide in-situ reinforced titanium and titanium alloy stent according to claim 1, wherein in the step 2, the mass of the sucrose accounts for 5-20% of the mass of the titanium source powder, and the mass of the graphene accounts for 0.5-4% of the mass of the titanium source powder.
5. The method for preparing the titanium carbide in-situ reinforced titanium and titanium alloy stent according to claim 1, wherein in the step 3, the freezing temperature is-120 ℃ to-30 ℃, the cooling rate is 5 to 15 μm/s, and the freezing time is 1.5 to 3 hours.
6. The method for preparing the titanium carbide in-situ reinforced titanium and titanium alloy stent as claimed in claim 1, wherein in the step 3, the bottom of the mold is made of heat conducting material, and the heat conducting material is aluminum, copper or silver.
7. The method for preparing the titanium carbide in-situ reinforced titanium and titanium alloy stent according to claim 1, wherein in the step 3, the pressure of the low-pressure environment is 10-100 Pa.
8. The method for preparing the titanium carbide in-situ reinforced titanium and titanium alloy stent according to claim 2, wherein in the step 4, the sintering temperature is 1200-1400 ℃ and the sintering time is 1.5-3 h.
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| CN112342419B (en) * | 2020-09-23 | 2022-04-15 | 华南理工大学 | Method for preparing TiC reinforced titanium-based composite material based on cross-linked modified sintered titanium hydride |
| CN112517910A (en) * | 2020-11-13 | 2021-03-19 | 西安理工大学 | Method for improving strength of high-porosity layered porous titanium and titanium alloy |
| CN112553494B (en) * | 2020-11-13 | 2022-03-01 | 南京航空航天大学 | Refrigeration device and method for preparing high-strength and high-toughness layered porous titanium alloy material by using same |
| CN113182520B (en) * | 2021-03-31 | 2022-09-02 | 北京科技大学 | Titanium product with titanium carbide reinforced titanium-based composite material hardened layer and preparation method |
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Effective date of registration: 20211227 Address after: 241000 building 7, Beihang Wuhu TONGHANG Innovation Park, Anhui Xinwu Economic Development Zone, Wanhe District, Wuhu City, Anhui Province Patentee after: Anhui yuehuihui Intelligent Equipment Co.,Ltd. Address before: 710048 Shaanxi province Xi'an Beilin District Jinhua Road No. 5 Patentee before: XI'AN University OF TECHNOLOGY |