Porous ceramic material and processes for preparing same

• US 4,654,314 A
• Filed: 07/06/1984
• Issued: 03/31/1987
• Est. Priority Date: 07/09/1983
• Status: Expired due to Fees

• Current Assignee: Sumitomo Chemical Company Limited
• Original Assignee: Sumitomo Chemical Company Limited
• Inventors: Yamauchi, Shigeru, Takagi, Shigehide
• Primary Examiner(s): NOT, DEFINED
• Assistant Examiner(s): Capella, Steven
• Application Number:
  US06/628,600
• Time in Patent Office: 998 Days
• Field of Search: 501/80, 501/82, 501/83, 501/85, 501/1, 264/44, 128/92 C, 3/1.9
• US Class Current: 501/82
• CPC Class Codes: A61F 2310/00293 containing a phosphorus-containing compound, e.g. apatite
• CPC Class Codes: A61L 2400/18 Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
• CPC Class Codes: A61L 27/12 Phosphorus-containing materials, e.g. apatite
• CPC Class Codes: A61L 27/56 Porous materials, e.g. foams or sponges
• CPC Class Codes: C04B 2111/00836 for medical or dental applications
• CPC Class Codes: C04B 2111/00844 for electronic applications
• CPC Class Codes: C04B 33/24 Manufacture of porcelain or white ware
• CPC Class Codes: C04B 38/0051 characterised by the pore size, pore shape or kind of porosity
• CPC Class Codes: C04B 38/065 characterised by physical aspects, e.g. shape, size or porosity
• CPC Class Codes: C04B 38/067 Macromolecular compounds C04B38/062 takes precedence; polysaccharides C04B38/0645
• CPC Class Codes: C04B 38/106 by adding preformed foams

Abstract

A porous ceramic material composed of a sintered porous body of a calcium phosphate compound is described. A multiplicity of capillary void paths having a diameter of 1 to 30 μm and a multiplicity of pores having a diameter of 1 to 600 μm are formed in the sintered porous body. At least part of the pores are connected to the exterior space of the sintered porous body through at least a part of the capillary voids. The porous ceramic material is valuable as a medical material, e.g., a substitute or prosthesis for bone or dental root, and also an electronic material and a genetic engineering material.

When the porous ceramic material is embedded in a bone defect of human or animals, osteolytic cells, osteoblasts, erythrocytes and body fluid are selectively allowed to intrude through the porous ceramic material while almost no intrusion of osteoclasts and collagen fibers is allowed. Accordingly, the porous ceramic material can be utilized for inducing new-born bone, controlling resorption of bone with age, remedying bone defects.

Claims

1. A process for the preparation of a porous ceramic material, which comprises the steps of:

bubbling 100 parts by weight of albument to form a multiplicity of bubbles having a size of 1 to 600 μ

m;

incorporating the bubbled albumen with 30 to 120 parts by weight of a calcium phosphate compound powder and 1 to 5 parts by weight of an organic fiber having a length of 5 μ

m to 5 mm and a diameter of 1 to 30 μ

m,

shaping the thus-obtained mixture into a desired shape and size,

heating the shaped mixture at a temperature of 120°

to 150°

C. to harden the albumen;

heating the hardened shaped mixture at a temperature of 500°

to 700°

C. to carbonize the hardened albumen and organic fiber; and

then,

heating the carbonized shaped mixture at a temperature of 800°

to 2,350°

C. in an oxygen-containing atmosphere to remove the carbonization product by burning and to sinter the calcium phosphate compound powder.

2. A process according to claim 1, wherein the step of heating the shaped mixture for the hardening of albumen is carried out in an atmosphere having a relative humidity of 30 to 70% at a temperature-elevating rate of 5°

to 10°

C./min.

3. A process according in claim 1, wherein the calcium phosphate compound powder has a particle diameter 0.05 to 10 μ

m.

4. A process according to claim 1, wherein the organic fiber is at least one member selected from an animal fiber, a silk fiber, a cellulose fiber and an organic synthetic fiber.

5. A process for the preparation of a porous ceramic material, which comprises the steps of:

mixing 20 to 300 parts by weight of sublimable solid substance particles having a particle diameter of 1 to 600 μ

m and 1 to 5 parts by weight of an organic fiber having a length of 5 μ

m to 5 mm and a diameter of 1 to 30 μ

m with 100 parts by weight of a calcium phosphate compound powder;

press-shaping the thus-obtained mixture into a desired shape and size;

heating the shaped mixture at a temperature of 200°

to 800°

C. to remove the sublimable substance by sublimation and carbonize the organic fiber; and

then,

heating the shaped mixture at a temperature of 800°

to 1,350°

C. in an oxygen-containing atmosphere to remove the carbonization product by burning and sinter the calcium phosphate compound powder.

6. A process according to claim 5, wherein the calcium phosphate compound powder has a particle diameter of 0.05 to 10 μ

m.

7. A process according to claim 5, wherein the sublimable solid substance is at least one member selected from the group consisting of camphor, menthol and naphthalene.

8. A process according to claim 5, wherein the organic fiber is at least one member selected from the group consisting of an animal fiber, a silk fiber, a cellulose fiber and an organic synthetic fiber.

9. A process for the preparation of a porous ceramic material, which comprises the steps of:

mixing 25 to 380 parts by weight of organic synthetic resin particles having a particle diameter of 1 to 600 μ

m and 1 to 5 parts by weight of an organic fiber having a length of 5 μ

m to 5 mm and a diameter of 1 to 30 μ

m with 100 parts by weight of a calcium phosphate compound powder;

press-shaping the thus-obtained mixture into a desired shape and size;

heating the shaped mixture at a temperature of 200°

to 800°

C. to remove the organic synthetic resin by thermal decomposition and carbonize the organic fiber; and

then,

heating the shaped mixture at a temperature of 800°

to 1,350°

C. in an oxygen-containing atmosphere to remove the carbonization product by burning and sinter the calcium phosphate compound powder.

10. A process according to claim 9, wherein the calcium phosphate compound powder has a particle diameter of 0.05 to 10 μ

m.

11. A process according to claim 9, wherein the organic synthetic resin is at least one member selected from the group consisting of polymethyl methacrylate, polypropyelne and polystyrene.

12. A process according to claim 9, wherein the organic fiber is at least one member selected from the group consisting of an animal fiber, a silk fiber, a cellulose fiber and an organic synthetic fiber.

13. A process according to claim 9, wherein the organic synthetic resin particles have a particle diameter of 10 to 300 μ

m.

14. A process for the preparation of a porous ceramic material, which comprises the steps of:

mixing 25 to 380 parts by weight of organic synthetic resin particles having a particle diameter of 1 to 600 μ

m, 2 to 5 parts by weight of sublimable solid substance particles having a particle diameter of 1 to 600 μ

m and 1 to 5 parts by weight of an organic fiber having a length of 5 μ

m to 5 mm and a diameter of 1 to 30 μ

m with 100 parts by weight of a calcium phosphate compound powder;

press-shaping the thus-obtained mixture into a desired shape and size;

heating the shaped mixture at a temperature of 200°

to 800°

C. to remove the organic synthetic resin particles by thermal decomposition, carbonize the organic fiber and remove the sublimable substance particles by sublimation; and

then,

heating the shaped mixture at a temperature of 800°

to 1,350°

C. in an oxygen-containing atmosphere to remove the carbonization product by burning and sinter the calcium phosphate compound powder.

15. A process according to claim 14, wherein the sublimable substance is at least one member selected from the group consisting of camphor, menthol and naphthalene.

16. A process according to claim 15, wherein the organic synthetic resin particles have a particle diameter of to 300 μ

m.

17. A process according to claim 14, wherein the organic synthetic particles have a particle diameter of 10 to 300 μ

m.