CN113200748B - Boron nitride-diamond-zirconia hybrid composite material and preparation method thereof - Google Patents

Boron nitride-diamond-zirconia hybrid composite material and preparation method thereof Download PDF

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CN113200748B
CN113200748B CN202110418617.5A CN202110418617A CN113200748B CN 113200748 B CN113200748 B CN 113200748B CN 202110418617 A CN202110418617 A CN 202110418617A CN 113200748 B CN113200748 B CN 113200748B
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boron nitride
diamond
zirconia
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CN113200748A (en
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张旺玺
刘书锋
崔卫民
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Zhengzhou Berlt Hard Materials Co ltd
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Abstract

The invention provides a boron nitride-diamond-zirconia hybrid composite material and a preparation method thereof, wherein the boron nitride-diamond-zirconia hybrid composite material comprises the following raw materials in parts by weight: 15-75 parts of boron nitride micro powder, 10-50 parts of diamond micro powder, 10-30 parts of zirconia micro powder and 10-20 parts of titanium powder. Firstly, mixing and ball milling boron nitride, diamond and zirconia powder with specific granularity, putting the mixed powder into a ceramic crucible, sintering the mixed powder in a muffle furnace to 700 ℃, mixing the mixed powder with bioactive titanium powder, putting the mixed powder into an assembly block, and putting the assembly block into a hexahedral top press for synthesis under high pressure to obtain the compact sintered body of the boron nitride-diamond-zirconia hybrid composite ceramic material. The invention has the characteristics of high hardness, good toughness, good biocompatibility and the like of the synthesized bone implant material, and particularly the physicochemical properties of the materials can be arbitrarily designed by changing the proportion of the raw materials of boron nitride, diamond and zirconia, so that the proper hardness, strength and toughness can be obtained.

Description

Boron nitride-diamond-zirconia hybrid composite material and preparation method thereof
Technical Field
The invention relates to the technical field of hard biological material preparation, in particular to a boron nitride-diamond-zirconia hybrid composite material and a preparation method thereof.
Background
The ideal orthopedic implant material needs to have sufficient hardness, proper strength and physical and chemical properties, and sufficient loading capacity, wear resistance and corrosion resistance in addition to excellent biocompatibility and bioactivity. In general, the following requirements are required: (1) In terms of biological performance, the biological tissue compatibility is required to be good, the mechanical compatibility, namely the biological binding property is good, and the biological tissue adhesive has no adverse effect, no rejection and no toxic or side effect on surrounding bone tissues. (2) In the aspect of physical and chemical properties, the material is required to have definite chemical components, stable mechanical properties and surface properties and wear resistance. The anti-corrosion and fatigue resistance are good, the anti-corrosion and fatigue resistance can not lose efficacy due to electrochemical and chemical corrosion in human body environment, and the anti-corrosion and fatigue resistance can not be damaged under the action of human body cycle fatigue.
The main raw materials of the orthopedic implant meeting the requirements comprise ceramics, titanium alloy, forged titanium alloy, cast cobalt-chromium-molybdenum alloy and medical ultra-high molecular weight polyethylene material. Each of these materials has its own characteristics. Stainless steel is used as an implant material for a thin film joint or a bone plate at the earliest time, has excellent processability and enough strength and toughness, but has the problems of poor corrosion resistance, easy aging and poor biocompatibility in clinical use, and metal ions generated by abrasion are harmful to human bodies. Titanium alloy has the characteristics of low relative density, high strength, good ductility, corrosion resistance, fatigue resistance and the like, but is easy to wear, and metal ions and particles generated by wear have potential toxicity. Bioceramics, such as alumina and zirconia ceramics, are relatively stable in structure, have relatively high strength, wear resistance and chemical stability, can avoid the problem that metal ions are easily released from metal prostheses, and zirconia has more excellent fracture strength than alumina, but the zirconia ceramics are relatively low in hardness. Carbon materials have proven to be well compatible with living beings, and carbon fiber reinforced composites are therefore used in many applications, but the non-carbon components of carbon fiber composites are disadvantageous.
To address the different problems that occur with different materials, researchers have employed a variety of approaches. Some emphasis is placed on the modification of materials or the design of composite structures, and some on the synthesis and preparation of new materials. In order to solve the problem that the elastic modulus of the bionic bone of the titanium alloy is not matched with that of the human bone, the titanium alloy implant with a porous structure is adopted by the university of south China Chen Ke and the like to adapt to the mechanical property of the human bone (Chen Ke, yun Zhong and the like. Chinese patent (application number 202010918664.1) discloses a preparation method and application of an alumina-based metal composite ceramic bone implant prosthesis, which are mainly used for enhancing the toughness of composite ceramics and widening the application field of the composite ceramics. Chinese patent (application No. 202011036722.4) discloses a preparation method of profiling artificial bone of carbon fiber composite material, which comprises mixing carbon fiber with polymer fiber, braiding, hot pressing to decompose and remove organic components, and depositing diamond-like carbon coating on the surface by chemical vapor deposition. However, none of these approaches fundamentally address adequate wear resistance, chemical stability and biocompatibility issues. For example, the porous titanium alloy and alumina-based metal composite ceramic bone implant prosthesis still has certain metal ion infiltration toxicity after abrasion; the hardness of the bone implant material coated with diamond after the carbon fiber and the polymer fiber are mixed and woven is insufficient.
Disclosure of Invention
The invention provides a preparation method of a boron nitride-diamond-zirconia hybrid composite material, which can fully utilize the characteristics of compact material structure and high hardness prepared under high pressure, and overcomes the defects that the material components are single or the advantages of the material components can not be fully exerted when the materials are compounded in the existing method, and the hardness, toughness and other main properties of the material are difficult to regulate and control.
The technical scheme for realizing the invention is as follows:
the boron nitride-diamond-zirconia hybrid composite material comprises the following raw materials in parts by weight: 15-75 parts of boron nitride micro powder, 10-50 parts of diamond micro powder, 10-30 parts of zirconia micro powder and 10-20 parts of titanium powder.
Preferably, the feed comprises the following raw materials in parts by weight: 50 parts of boron nitride micro powder, 30 parts of diamond micro powder, 15 parts of zirconia micro powder and 5 parts of titanium powder.
The boron nitride micro powder is one of hexagonal boron nitride or cubic boron nitride; the granularity of the boron nitride micro powder is 50-200 nm; the granularity of the diamond micro powder is 100-200 nm; the granularity of the zirconia micropowder is 20-100 nm; before use, the titanium powder is purified to avoid forming dense oxide impurity on the surface, the purity is up to 99.99%, and the granularity of the titanium powder is 10-50 μm.
A process for preparing the compact sintered body of boron nitride-diamond-zirconium oxide hybridized composite ceramic material includes such steps as mixing the boron nitride, diamond and zirconium oxide powder with specific granularity (coarse granularity, poor uniformity of composite structure, low strength, and easy aggregation of fine granularity powder and oxidization of surface), ball grinding, loading in ceramic crucible, sintering to 700-800 deg.C, mixing with bioactive titanium powder, loading in assembling block, and high-pressure synthesizing.
The method comprises the following specific steps:
(1) Mixing and ball milling: mixing diamond micropowder, boron nitride micropowder and zirconia micropowder according to a certain mass ratio, and ball-milling by using a sand mill, wherein the ball-milling medium is acetone;
(2) Vacuum heat treatment: carrying out heat treatment on the mixture of the mixture diamond micropowder, the boron nitride micropowder and the zirconia micropowder obtained in the step (1) in a vacuum muffle furnace at 700-800 ℃ for 1-2h;
(3) Adding titanium powder: adding titanium powder into the diamond micro powder, boron nitride micro powder and zirconia micro powder mixture subjected to heat treatment in the step (2), and uniformly mixing under vacuum or nitrogen protection atmosphere to form a pre-synthesis premix;
(4) And (3) assembling a synthesis block: weighing and assembling the premix obtained in the step (3) into a synthetic block;
(5) High-pressure synthesis: and (3) putting the synthesized block obtained in the step (4) into a hexahedral press, synthesizing at high pressure and high temperature for 20-30 min, wherein the synthesis pressure is 4-5 GPa, the temperature is 900-1400 ℃, and taking out after cooling to obtain the composite ceramic material.
The beneficial effects of the invention are as follows: the invention has the characteristics of high hardness, good toughness, good biocompatibility and the like of the synthesized bone implant material, and particularly the physicochemical properties of the materials can be arbitrarily designed by changing the proportion of the raw materials of boron nitride, diamond and zirconia, so that the proper hardness, strength and toughness can be obtained. Meanwhile, the size of the high-pressure synthesis cavity of the large-cavity hexahedral press manufactured by the large-scale forging technology is enough to synthesize a large-size block material, the large-size block material is cut into a required shape by laser or electric spark, and the boron nitride-diamond-zirconia hybrid composite ceramic material compact sintered body is obtained after polishing, so that the large-size hexahedral press has great economic and social benefits.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without any inventive effort, are intended to be within the scope of the invention.
Example 1
The compact sintered body of the boron nitride-diamond-zirconia hybrid composite ceramic material is prepared by synthesizing the following components in parts by weight: boron nitride micropowder 50; diamond micropowder 30; zirconia micropowder 15; titanium powder 5.
The method comprises the following steps:
step 1, mixing and ball milling: mixing diamond micropowder, hexagonal boron nitride micropowder and zirconia micropowder according to the mass ratio, and performing ball milling by using a sand mill, wherein a ball milling medium is acetone, and the ball milling time is 6 h;
step 2, vacuum heat treatment: carrying out heat treatment on the mixture of the diamond micro powder, the hexagonal boron nitride micro powder and the zirconia micro powder obtained in the step 1 in a vacuum muffle furnace at 700 ℃ for 1.5 h;
step 3, adding titanium powder: adding the balance of titanium powder into the diamond micropowder, hexagonal boron nitride micropowder and zirconia micropowder mixture subjected to the heat treatment in the step 2, and uniformly mixing under the protection of nitrogen to form a pre-synthesis premix;
step 4, assembling a synthesis block: weighing and assembling the premix obtained in the step 3 into a synthetic block;
step 5, high-pressure synthesis: putting the synthesized block obtained in the step 4 into a hexahedral top press, synthesizing for 25 min at the high temperature of 1100 ℃ under the synthesis pressure of 4.5 GPa, cooling, taking out, and performing laser cutting, grinding and polishing to obtain a compact sintered body of the boron nitride-diamond-zirconia hybrid composite ceramic material with the required shape, wherein the mechanical strength of the compact body reaches 320.77 MPa, the Young modulus reaches 21.91 MPa and the density is 2.61 g/cm 3 。
Example 2
The compact sintered body of the boron nitride-diamond-zirconia hybrid composite ceramic material is prepared by synthesizing the following components in parts by weight: boron nitride micropowder 40; diamond micropowder 40; zirconia micropowder 10; titanium powder 10.
The method comprises the following steps:
step 1, mixing and ball milling: mixing diamond micropowder, cubic boron nitride micropowder and zirconia micropowder according to a certain mass ratio, ball-milling by using a sand mill, wherein the ball-milling medium is acetone, and the ball-milling time is 6 h.
Step 2, vacuum heat treatment: the diamond micropowder, cubic boron nitride micropowder and zirconia micropowder mixture obtained in step 1 was heat-treated in a vacuum muffle furnace at 750 ℃ for 1 h.
Step 3, adding titanium powder: and (2) adding the balance of titanium powder into the diamond micropowder, cubic boron nitride micropowder and zirconia micropowder mixture subjected to the heat treatment in the step (2), and uniformly mixing under the protection of nitrogen to form the pre-synthesis premix.
Step 4, assembling a synthesis block: and (3) weighing and assembling the premix obtained in the step (3) into a synthetic block.
Step 5, high-pressure synthesis, namely placing the synthesized block obtained in the step 4 into a hexahedral top press, synthesizing for 25 minutes under the conditions of synthesis pressure of 4 GPa and temperature of 1000 ℃, cooling, taking out, and then performing laser cutting, grinding and polishing to obtain a compact sintered body of the boron nitride-diamond-zirconia hybrid composite ceramic material with the required shape, wherein the mechanical strength of the compact body reaches 331.43 MPa, the Young modulus reaches 23.65 MPa, and the density is 2.72 g/cm 3 。
Example 3
The compact sintered body of the boron nitride-diamond-zirconia hybrid composite ceramic material is prepared by synthesizing the following components in parts by weight: boron nitride micropowder 75; diamond micropowder 50; zirconia micropowder 30; titanium powder 20.
The method comprises the following steps:
step 1, mixing and ball milling: mixing diamond micropowder, cubic boron nitride micropowder and zirconia micropowder according to a certain mass ratio, ball-milling by using a sand mill, wherein the ball-milling medium is acetone, and the ball-milling time is 6 h.
Step 2, vacuum heat treatment: and (2) carrying out heat treatment on the diamond micropowder, cubic boron nitride micropowder and zirconia micropowder mixture obtained in the step (1) in a vacuum muffle furnace at 800 ℃ for 2 h.
Step 3, adding titanium powder: and (2) adding the balance of titanium powder into the diamond micropowder, cubic boron nitride micropowder and zirconia micropowder mixture subjected to the heat treatment in the step (2), and uniformly mixing under the protection of nitrogen to form the pre-synthesis premix.
Step 4, assembling a synthesis block: and (3) weighing and assembling the premix obtained in the step (3) into a synthetic block.
And 5, high-pressure synthesis, namely placing the synthesized block obtained in the step 4 into a hexahedral press, synthesizing for 25 minutes under the conditions of synthesis pressure of 5 GPa and temperature of 900 ℃, cooling, taking out, and performing laser cutting, grinding and polishing to obtain the boron nitride-diamond-zirconia hybrid composite ceramic material compact sintered body with the required shape.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.

Claims (3)

1. The boron nitride-diamond-zirconia hybrid composite material is characterized by comprising the following raw materials in parts by weight: 15-75 parts of boron nitride micro powder, 10-50 parts of diamond micro powder, 10-30 parts of zirconia micro powder and 10-20 parts of titanium powder; the boron nitride micro powder is one of hexagonal boron nitride or cubic boron nitride; the granularity of the boron nitride micro powder is 50-200 nm; the granularity of the diamond micro powder is 100-200 nm; the granularity of the zirconia micropowder is 20-100 nm; the granularity of the titanium powder is 10-50 mu m;
the preparation method of the boron nitride-diamond-zirconia hybrid composite material comprises the following steps:
(1) Mixing and ball milling: mixing diamond micropowder, boron nitride micropowder and zirconia micropowder for ball milling;
(2) Vacuum heat treatment: carrying out vacuum heat treatment on the mixture obtained in the step (1);
(3) Adding titanium powder: adding titanium powder into the mixture subjected to the heat treatment in the step (2), and uniformly mixing under vacuum or nitrogen protection atmosphere to form a premix;
(4) And (3) assembling a synthesis block: weighing and assembling the premix obtained in the step (3) into a synthetic block;
(5) High-pressure synthesis: putting the synthesized block obtained in the step (4) into a hexahedral press, synthesizing at high pressure and high temperature, cooling, and taking out to obtain a composite ceramic material;
the temperature of the vacuum heat treatment in the step (2) is 700-800 ℃ and the time is 1-2h;
the synthesis pressure in the step (5) is 4-5 GPa, and the temperature is 900-1400 ℃.
2. The boron nitride-diamond-zirconia hybrid composite material according to claim 1, comprising the following raw materials in parts by weight: 50 parts of boron nitride micro powder, 30 parts of diamond micro powder, 15 parts of zirconia micro powder and 5 parts of titanium powder.
3. A boron nitride-diamond-zirconia hybrid composite material according to claim 1 or 2, characterized in that: and (3) ball milling is carried out by using a sand mill in the step (1), wherein the ball milling medium is acetone.
CN202110418617.5A 2021-04-19 2021-04-19 Boron nitride-diamond-zirconia hybrid composite material and preparation method thereof Active CN113200748B (en)

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