Degradable self-reinforced zinc-based composite material, preparation method and intervertebral fusion cage

Abstract

The present application relates to a kind of degradable self-reinforced zinc-based composite, preparation method and intervertebral fusion cage, and the component and the mass percentage of each component of degradable self-reinforced zinc-based composite are as follows: 0wt% < iron-rich phase ≤15wt%, 0wt% < manganese-rich phase ≤5wt%, 80wt% ≤Zn <100wt%;Wherein, the 50wt% ≤Fe <100wt% in the iron-rich phase, 80wt% ≤Mn <100wt% in manganese-rich phase.The preparation method includes nodular graphite powder mixing, ordinary powder mixing, injection molding and debinding sintering.The interface of the degradable self-reinforced zinc-based composite of the present application is stable, and can be molded into the part of intervertebral fusion cage in the preparation process.

Description

Technical Field

[0001] This invention relates to the field of medical metal composite materials, specifically to a biodegradable self-reinforced zinc-based composite material, its preparation method, and an interbody fusion device. Background Technology

[0002] Medical materials can be classified according to their composition and properties into medical metallic materials, medical polymer materials, medical ceramic materials, medical composite materials, and their derivative materials. Among them, medical metallic composite materials are gradually increasing in actual clinical applications due to their excellent mechanical and processing properties. Moreover, medical metallic composite materials with biodegradable properties can more effectively reduce the damage caused by secondary surgeries compared to conventional bio-inert materials.

[0003] Degenerative spinal diseases are common and frequently occurring diseases in orthopedics, mainly including intervertebral disc degeneration, spinal stenosis, spondylolisthesis, and compression of the spinal cord or nerve roots. Interbody fusion is a commonly used and effective treatment for these diseases. As an important component of interbody fusion surgery, the interbody fusion device mainly functions to restore the intervertebral space height and the normal physiological curvature of the vertebral bodies, achieve immediate postoperative stability, and promote bony fusion of the intervertebral spaces.

[0004] Therefore, using medical metal composite materials to prepare interbody fusion devices is a good option. However, due to the limitations of traditional medical composite material preparation processes, existing medical composite materials are difficult to mold into parts for interbody fusion devices during the preparation process and require post-processing, which brings great inconvenience to the manufacturing of interbody fusion devices. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to overcome the defects of the prior art and provide a biodegradable self-reinforced zinc-based composite material with stable interface and which can be molded into parts of intervertebral fusion device during the preparation process.

[0006] To solve the above-mentioned technical problems, the technical solution of the present invention is: a biodegradable self-reinforced zinc-based composite material, wherein the components and the mass percentage of each component are as follows:

[0007] 0wt% < iron-rich phase ≤ 15wt%, 0wt% < manganese-rich phase ≤ 5wt%, 80wt% ≤ Zn < 100wt%; among which,

[0008] The iron-rich phase contains 50wt% ≤ Fe < 100wt%, and the manganese-rich phase contains 80wt% ≤ Mn < 100wt%.

[0009] This invention also provides a method for preparing a biodegradable, self-reinforced zinc-based composite material, the method comprising:

[0010] S1, Ball milling and mixing: Weigh zinc powder, iron powder and manganese powder according to atomic percentage, mix them and seal them in a ball milling jar, and ball mill them to obtain a mixed powder of self-generated particle reinforcement phase and zinc matrix;

[0011] S2, Ordinary powder mixing: The powder mixture of the self-generated particle reinforcing phase and zinc matrix is ​​mixed evenly with the binder to obtain a mixture;

[0012] S3, Injection molding: The mixture is heated and injected into a part mold and held under pressure to obtain a part preform;

[0013] S4, Degreasing and Sintering: The part preform is subjected to a heat preservation degreasing and sintering process in an inert atmosphere to obtain the part.

[0014] Furthermore, the binder includes one of tetrahydrofuran, dextrin, starch, aluminum hydroxyl sol, cyanoacrylate, and furan resin.

[0015] Furthermore, in S3, the heating temperature is 60-120℃, the injection pressure is 70-100MPa, and the holding time is 300-600s.

[0016] Furthermore, in S4, during the heat preservation and degreasing process, the vacuum level is adjusted to be below 10. -4 Pa, heated to 150-450 ℃ at a heating rate of 10-30 ℃ / min, and held at that temperature for 60-180 min.

[0017] Furthermore, in S4, during the sintering process, argon gas with a purity of 99.9% is introduced as a protective gas, the sintering pressure is controlled at 30~40MPa, the sintering temperature is 400~850℃, and the sintering time is 10~60 min.

[0018] The present invention also provides an intervertebral fusion device, wherein all its parts are made of biodegradable self-reinforced zinc-based composite material, or wherein all its parts are made of biodegradable self-reinforced zinc-based composite material prepared by a method thereof.

[0019] The present invention also provides an interbody fusion device, comprising a main body, an upper cover, a lower cover, two sets of upper support rods, two sets of lower support rods, two drive rods, and four screw-on handles; wherein,

[0020] Each end of the upper cover is hinged to the upper end of a set of upper support rods;

[0021] Each end of the lower cover is hinged to the lower end of a set of lower support rods;

[0022] Each drive rod is rotatably connected to the lower end of the upper support rod and the upper end of the lower support rod, which are located at the same end.

[0023] The main body is provided with a horizontal slide groove, and the drive rod is slidably installed in the horizontal slide groove. The two drive rods are used to drive the upper cover and the lower cover to close together when moving towards each other along the horizontal slide groove, and to drive the upper cover and the lower cover to open when moving away from each other along the horizontal slide groove.

[0024] Each end of the drive rod is threadedly connected to the screwing handle, which is used to lock the positions of the upper support rod and the lower support rod when screwed to abut against the body.

[0025] Furthermore, the intervertebral fusion device also includes a screw, which is threadedly connected to the main body and has its head rotatably connected to a drive rod. The screw is used to drive the drive rod to slide along the horizontal groove during its screwing in or out.

[0026] Furthermore, the upper cover and the lower cover are each equipped with a pressure sensor.

[0027] By adopting the above technical solution, the present invention has the following beneficial effects:

[0028] The biodegradable self-reinforced zinc-based composite material of the present invention has two self-reinforced particle phases, which can effectively strengthen the alloy matrix and improve the interfacial stability in the microstructure of the alloy matrix. It has excellent strength, wear resistance and microstructure stability.

[0029] The method for preparing the biodegradable self-reinforced zinc-based composite material in this invention can directly form the parts of the intervertebral fusion device during the preparation process, which facilitates the subsequent preparation of the intervertebral fusion device. Moreover, the entire preparation method has fewer steps and is easy to operate.

[0030] The interbody fusion device in this invention can be height-adjusted during surgery and can be locked. After surgery, the implantation status can be observed through data transmitted by pressure sensors, which is convenient and saves time. Attached Figure Description

[0031] Figure 1 The microstructure of the zinc-based composite material (11 wt.% iron-rich phase and 3 wt.% manganese-rich phase) was observed by SEM.

[0032] Figure 2 The hardness of the zinc-based composite material (11 wt.% iron-rich phase and 3 wt.% manganese-rich phase) obtained by Vickers hardness testing;

[0033] Figure 3 The microstructure of the zinc-based composite material (15 wt.% iron-rich phase and 5 wt.% manganese-rich phase) was observed by SEM.

[0034] Figure 4The hardness of the zinc-based composite material (15 wt.% iron-rich phase and 5 wt.% manganese-rich phase) obtained by Vickers hardness testing;

[0035] Figure 5 This is an isometric view of the interbody fusion device in this invention;

[0036] Figure 6 This is a front view of the interbody fusion device in this invention;

[0037] Figure 7 This is an exploded view of the interbody fusion device in this invention;

[0038] Figure 8 This is a schematic diagram of the upper support rod in this invention;

[0039] Figure 9 This is a schematic diagram of the lower support rod in this invention;

[0040] Figure 10 This is a schematic diagram of the main body of the present invention;

[0041] Figure 11 This is a top view of the main body of the present invention;

[0042] Figure 12 This is a schematic diagram of the structure in which a pressure sensor is mounted on the top cover in this invention;

[0043] In the diagram, 1. Top cover; 11. Top cover through hole; 2. Upper support rod; 21. Upper support rod upper through hole; 22. Upper support rod lower through hole; 3. Main body; 31. Threaded hole; 32. Horizontal slide groove; 33. First partition plate; 34. Cross block; 35. Second partition plate; 4. Fixing rod; 5. Countersunk screw; 6. Drive rod; 7. Lower support rod; 71. Lower support rod lower through hole; 72. Lower support rod upper through hole; 8. Screw; 9. Tightening handle; 10. Lower cover; 110. Pressure sensor; 120. Transmission assembly. Detailed Implementation

[0044] To make the content of this invention easier to understand, the invention will be further described in detail below with reference to specific embodiments and accompanying drawings.

[0045] Example 1

[0046] A biodegradable, self-reinforced zinc-based composite material, comprising the following components and their mass percentages:

[0047] 0 wt% < iron-rich phase ≤ 15 wt%, 0 wt% < manganese-rich phase ≤ 5 wt%, balance is zinc; among which,

[0048] In the iron-rich phase, 50wt%≤Fe<100wt% and in the manganese-rich phase, 80wt%≤Mn<100wt%

[0049] Example 2

[0050] (1) Pure zinc, pure iron and pure manganese were weighed in an atomic ratio of 80:15:5, and the mixed raw materials were sealed in a ball mill jar under an inert gas environment. Then, the mixture was ball milled in a planetary ball mill to obtain a mixed powder containing 11 wt.% of iron-rich phase (containing 78 wt.% of iron) and 3 wt.% of manganese-rich phase (containing 83 wt.% of manganese), with the remainder being zinc.

[0051] (2) Mix the above-mentioned mixed powder and furan resin evenly to obtain a mixture;

[0052] (3) After heating the mixture, inject it into the mold of the intervertebral fusion device parts and hold it under pressure. The heating temperature is 80 ℃, the injection pressure is 90 MPa, and the holding pressure is 300 s to obtain the preform of the parts;

[0053] (4) The prefabricated parts are heat-insulated and degreased under vacuum conditions, and the vacuum degree is adjusted to be lower than 10. -4 Pa, heated to 300 °C at a heating rate of 15 °C / min, and held at that temperature for 120 min;

[0054] (5) The part preform is sintered in an inert atmosphere, and argon gas with a purity of 99.9% is introduced as a protective gas. The sintering pressure is controlled at 30 MPa, the sintering temperature is 600 ℃, and the sintering time is 30 min to obtain the part.

[0055] It should be noted that furan resin will be removed during the heat preservation and degreasing process. The adhesive is only used to assist in molding in step (3). The part obtained in this embodiment can be used as a part of an interbody fusion device or as a part of other implantable devices.

[0056] Figure 1 The microstructure of the zinc-based composite material (11 wt.% iron-rich phase and 3 wt.% manganese-rich phase) was observed by SEM.

[0057] Figure 2 The hardness of the zinc-based composite material (11 wt.% iron-rich phase and 3 wt.% manganese-rich phase) was obtained by Vickers hardness testing.

[0058] Example 3

[0059] Pure zinc, pure iron, and pure manganese were weighed in an atomic ratio of 70:20:10. The mixed raw materials were sealed in a ball mill jar under an inert gas environment and then ball-milled in a planetary ball mill to obtain a mixed powder containing 15 wt.% iron-rich phase (containing 71 wt.% iron) and 5 wt.% manganese-rich phase (containing 87 wt.% manganese), with the remainder being zinc.

[0060] The above-mentioned mixed powder and dextrin are mixed evenly to obtain a mixture;

[0061] The mixture was heated and injected into the mold of the intervertebral fusion device parts and held under pressure. The heating temperature was 90 ℃, the injection pressure was 85 MPa, and the holding pressure was 420 s to obtain the preform of the part.

[0062] The preformed part is degreased under vacuum conditions, with the vacuum level adjusted to below 10. -4 Pa, heated to 400 ℃ at a heating rate of 20 ℃ / min, and held at that temperature for 100 min;

[0063] The preform of the part was sintered in an inert atmosphere, with 99.9% pure argon gas as a protective gas. The sintering pressure was controlled at 35 MPa, the sintering temperature at 650 ℃, and the sintering time was 45 min to obtain the part.

[0064] It should be noted that dextrin will be removed during the heat preservation and degreasing process. The adhesive is only used to assist in molding in step (3). The part obtained in this embodiment can be used as a part of an interbody fusion device or as a part of other implantable devices.

[0065] Figure 3 The microstructure of the zinc-based composite material (15 wt.% iron-rich phase and 5 wt.% manganese-rich phase) was observed by SEM.

[0066] Figure 4 The hardness of the zinc-based composite material (15 wt.% iron-rich phase and 5 wt.% manganese-rich phase) was obtained by Vickers hardness testing.

[0067] Example 4

[0068] An intervertebral fusion device, wherein all its parts are made of the biodegradable self-reinforced zinc-based composite material of Example 1, or wherein all its parts are made of the biodegradable self-reinforced zinc-based composite material prepared by the method of Example 2 or Example 3.

[0069] Example 5

[0070] Based on Example 4, such as Figure 5 , 6 As shown in figures 7, 8, 9, 10, 11, and 12, the interbody fusion device includes a main body 3, an upper cover 1, a lower cover 10, two sets of upper support rods 2, two sets of lower support rods 7, two drive rods 6, and four screw-on handles 9; among which,

[0071] Each end of the upper cover 1 is hinged to the upper end of a set of upper support rods 2;

[0072] Each end of the lower cover 10 is hinged to the lower end of a set of lower support rods 7;

[0073] Each drive rod 6 is rotatably connected to the lower end of the upper support rod 2 and the upper end of the lower support rod 7, which are located at the same end.

[0074] The main body 3 is provided with a horizontal slide groove 32, and the drive rod 6 is slidably installed in the horizontal slide groove 32. The two drive rods 6 are used to drive the upper cover 1 and the lower cover 10 to close together when moving towards each other along the horizontal slide groove 32, and to drive the upper cover 1 and the lower cover 10 to open when moving away from each other along the horizontal slide groove 32.

[0075] Each end of the drive rod 6 is threaded with a screw-on handle 9, which is used to lock the position of the upper support rod 2 and the lower support rod 7 when screwed to abut against the main body 3, so as to stabilize the intervertebral fusion device after implantation.

[0076] In this embodiment, as Figure 6 , 10 As shown, there are two horizontal sliding grooves 32 on each of the left and right side walls of the main body 3. One drive rod 6 is slidably fitted into the two horizontal sliding grooves 32 on the front side, and the other drive rod 6 is slidably fitted into the two horizontal sliding grooves 32 on the rear side.

[0077] In this embodiment, as Figure 7 , 8 As shown in Figure 9, each set of upper support rods 2 has two upper support rods 2, and each set of lower support rods 7 has two lower support rods 7. The upper support rod lower through holes 22 of each upper support rod 2 are arranged in two directions in the left and right direction. The lower support rod upper through hole 72 of each lower support rod 7 is one and is located between the two upper support rod lower through holes 22 of the corresponding upper support rod 2. The drive rod 6 passes through the corresponding upper support rod lower through hole 22 and lower support rod upper through hole 72.

[0078] In this embodiment, as Figure 10 , 11 As shown, the main body 3 is divided into two spaces, front and back, by a horizontal block 34. Each space is provided with two first partitions 33 and two second partitions 35. The first partitions 33 and the second partitions 35 are also provided with horizontal sliding grooves 32. The two first partitions 33 are spaced apart on the left and right sides of the corresponding space, and the two second partitions 35 are spaced apart between the two first partitions 33. The space between the first partitions 33 and the corresponding second partitions 35 is used for placing the upper support rod 2 and the lower support rod 7 on one side.

[0079] In this embodiment, as Figure 7As shown, the upper support rod 2 is hinged to the upper cover 1 via a fixing rod 4. The upper cover 1 has an upper cover through hole 11. The fixing rod 4 passes through both the upper support rod upper through hole 21 and the corresponding upper cover through hole 11. The upper cover through hole 1 and the upper support rod upper through hole 21 are coaxial, thus ensuring a tight fit between the upper support rod 2 and the upper cover 1. Similarly, the lower support rod 7 is hinged to the lower cover 10 via a fixing rod 4. The lower support rod 7 has a lower support rod lower through hole 71. The fixing rod 4 has an internal threaded hole with a smooth outer surface, and the inner hole can be connected and fixed with a countersunk screw 5.

[0080] Example 6

[0081] Based on Example 5, such as Figure 5 , 7 As shown, to better drive the movement of the upper support rod 2 and the lower support rod 7, the intervertebral fusion device may also include a screw 8, which is threadedly connected to the main body 3, and its head is rotatably connected to a drive rod 6. The screw 8 is used to drive the drive rod 6 to slide along the horizontal groove 32 during its screwing in or out. Figure 7 , 10 As shown, the main body 3 is provided with a threaded hole 31, and the screw 8 has an external thread, which is threadedly connected to the threaded hole 31 through its external thread.

[0082] Example 7

[0083] Based on Example 5 or Example 6, such as Figure 12 As shown, pressure sensors 110 are respectively provided on the upper cover 1 and the lower cover 10.

[0084] Specifically, during implantation, once the upper cover 1 and lower cover 10 achieve sufficient stress contact with the upper and lower endplates, this signal is received by the pressure sensor 110 and transmitted to the transmission component 120. After analysis by the transmission component 120, the data is transmitted to an external receiving device. Based on the transmitted values, it is determined whether there is perfect contact with the upper and lower endplates. Then, the screw handle 9 is tightened to shape the interbody fusion cage, ensuring a stable and perfect implantation of the fusion cage after implantation into the intervertebral space.

[0085] Post-surgery, data received from an external receiving device can be used to understand the implantation status of the intervertebral fusion device and determine whether it has settled, thus avoiding the need to use X-rays to determine the settlement status and reducing harm to the body.

[0086] Based on the above-described preferred embodiments of the present invention, and through the foregoing description, those skilled in the art can make various changes and modifications without departing from the inventive concept. The technical scope of this invention is not limited to the contents of the specification, but must be determined according to the scope of the claims.

Claims

1. A biodegradable, self-reinforced zinc-based composite material, characterized in that, Its components and the mass percentage of each component are as follows: The composition consists of 11 wt% iron-rich phase, 3 wt% manganese-rich phase, and the balance being Zn; among which... The iron-rich phase contains 50wt% ≤ Fe < 100wt%, and the manganese-rich phase contains 80wt% ≤ Mn < 100wt%. Preparation methods include: S1, Ball milling and mixing: Weigh zinc powder, iron powder and manganese powder according to atomic percentage, mix them and seal them in a ball milling jar, and ball mill them to obtain a mixed powder of self-generated particle reinforcement phase and zinc matrix; S2, Ordinary powder mixing: The powder mixture of the self-generated particle reinforcing phase and zinc matrix is ​​mixed evenly with the binder to obtain a mixture; S3, Injection molding: The mixture is heated and injected into a part mold and held under pressure to obtain a part preform; S4, Degreasing and Sintering: The part preform is subjected to a heat preservation degreasing and sintering process in an inert atmosphere to obtain the part; In S3, the heating temperature is 60-120℃, the injection pressure is 70-100MPa, and the holding time is 300-600s; In S4, during the heat preservation and degreasing process, the vacuum level is adjusted to be below 10. -4 Pa, heated to 150-450 ℃ at a heating rate of 10-30 ℃ / min, and held at that temperature for 60-180 min; In S4, during the sintering process, argon gas with a purity of 99.9% is introduced as a protective gas, the sintering pressure is controlled at 30~40MPa, the sintering temperature is 400~850℃, and the sintering time is 10~60 min.

2. The biodegradable self-reinforced zinc-based composite material according to claim 1, characterized in that, The binder includes one of tetrahydrofuran, dextrin, starch, aluminum hydroxyl sol, cyanoacrylate, and furan resin.

3. An interbody fusion device, characterized in that, All its parts are made of the biodegradable, self-reinforcing zinc-based composite material as described in claim 1 or 2.

4. The interbody fusion device according to claim 3, characterized in that, Includes a main body (3), an upper cover (1), a lower cover (10), two sets of upper support rods (2), two sets of lower support rods (7), two drive rods (6), and four screw-on handles (9); among which, Each end of the upper cover (1) is hinged to the upper end of a set of upper support rods (2); Each end of the lower cover (10) is hinged to the lower end of a set of lower support rods (7); Each drive rod (6) is rotatably connected to the lower end of the upper support rod (2) and the upper end of the lower support rod (7) located at the same end; The main body (3) is provided with a horizontal slide groove (32), and the drive rod (6) is slidably installed in the horizontal slide groove (32). The two drive rods (6) are used to drive the upper cover (1) and the lower cover (10) to close together when moving towards each other along the horizontal slide groove (32), and to drive the upper cover (1) and the lower cover (10) to open when moving away from each other along the horizontal slide groove (32). Each end of the drive rod (6) is threadedly connected to the screw rod (9), which is used to lock the position of the upper support rod (2) and the lower support rod (7) when screwed to abut against the body (3).

5. The interbody fusion device according to claim 4, characterized in that, It also includes a screw (8) which is threaded to the body (3) and whose head is rotatably connected to a drive rod (6). The screw (8) is used to drive the drive rod (6) to slide along the horizontal groove (32) during its screwing in or out.

6. The interbody fusion device according to claim 4, characterized in that, The upper cover (1) and the lower cover (10) are respectively equipped with pressure sensors (110).

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