CN1035443C - Potassium titanate crystal whiskers preparation method - Google Patents
Potassium titanate crystal whiskers preparation method Download PDFInfo
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- CN1035443C CN1035443C CN93111038A CN93111038A CN1035443C CN 1035443 C CN1035443 C CN 1035443C CN 93111038 A CN93111038 A CN 93111038A CN 93111038 A CN93111038 A CN 93111038A CN 1035443 C CN1035443 C CN 1035443C
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- potassium
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- potassium titanate
- titanium
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- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000013078 crystal Substances 0.000 title claims abstract description 13
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 22
- 239000011591 potassium Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 19
- 150000001875 compounds Chemical class 0.000 claims abstract description 18
- 239000010936 titanium Substances 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 8
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 230000007062 hydrolysis Effects 0.000 claims abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 239000010953 base metal Substances 0.000 claims description 2
- 229910001960 metal nitrate Inorganic materials 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 11
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 abstract description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 abstract description 5
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 abstract description 4
- 239000004323 potassium nitrate Substances 0.000 abstract description 4
- 235000010333 potassium nitrate Nutrition 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 3
- 238000010924 continuous production Methods 0.000 abstract description 2
- 239000001103 potassium chloride Substances 0.000 abstract description 2
- 235000011164 potassium chloride Nutrition 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract 1
- 229910001514 alkali metal chloride Inorganic materials 0.000 abstract 1
- 229910001963 alkali metal nitrate Inorganic materials 0.000 abstract 1
- 229910052936 alkali metal sulfate Inorganic materials 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- -1 etc. Substances 0.000 abstract 1
- 229910000027 potassium carbonate Inorganic materials 0.000 abstract 1
- 235000011181 potassium carbonates Nutrition 0.000 abstract 1
- 235000011118 potassium hydroxide Nutrition 0.000 abstract 1
- 229910001773 titanium mineral Inorganic materials 0.000 abstract 1
- 239000001038 titanium pigment Substances 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 15
- 238000002425 crystallisation Methods 0.000 description 10
- 238000001816 cooling Methods 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910010413 TiO 2 Inorganic materials 0.000 description 5
- 238000007669 thermal treatment Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 2
- 239000010425 asbestos Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- 235000015320 potassium carbonate Nutrition 0.000 description 2
- 229910052895 riebeckite Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920013657 polymer matrix composite Polymers 0.000 description 1
- 239000011160 polymer matrix composite Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000001778 solid-state sintering Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The present invention relates to a preparation method for preparing crystal whiskers of potassium titanate. Titanium containing compounds, such as rutile type titanium mineral powder, anatase, titanium pigment, etc., and potassium containing compounds, such as potassium hydroxide, potassium nitrate, potassium chloride, potassium carbonate, etc. are used as raw materials. The method is characterized in that one of alkali metal nitrate, sulfate and chloride, or a combination thereof is added to be used as a fluxing agent in a synthetic process. The method comprises the technological process that according to that the mole ratio of Ti: K is from 2 to 4:1, the raw materials are prepared, and 20 to 40 wt% of fluxing agent is simultaneously added to be mixed. At the temperature of 900 to 1300 DEG C, the mixture is synthesized for 30 minutes to 4 hours. Through hydrolysis, filtration and drying, the crystal whisker of potassium titanate is obtained. The method enhances the synthesis reaction efficiency and the crystal whisker quality, reduces the cost, and is convenient for industrial continuous production in batches.
Description
The present invention relates to the preparation method of Preparation of Whiskers technology, particularly potassium titanate crystal whisker.
Strengthen resin and metal with inorganic fibers,, come into one's own as high performance composite.Particularly POTASSIUM HEXATITANATE fiber can replace multiduty asbestos, avoids environmental pollution, more induces one to treat with special respect.But it is imperative to seek potassium titanate fiber manufacture method best in quality, suitability for industrialized production with low cost.
The method that in the past prepared potassium titanate fiber has hydrothermal method [1], sintering method [2], scorification [3], the gentle cold crystallization method [6] of quick cooling crystallization method [4.5] etc.But above-mentioned these preparation methods do not install, cost of equipment height, operate continuously difficulty; Burn till the genealogy of law raw mix is reacted synthon through solid state sintering, its resultant crystalline state is insufficient, and the fiber of generation is too short, has only several microns; The fusion genealogy of law is the raw mix high-temperature fusion, forms cooling curing crystallization again behind the melt.This method synthesis temperature height, the crystallization phases binding ratio of generation is tightr, and it is very difficult to separate fibre, and the diameter of gained fiber is bigger, generally greater than 10～30 μ m, and irregular, uniformity is poor, and it is bad to be used as the toughener effect; And the gentle cold crystallization method of quick cooling crystallization method all is to generate unsettled two potassium titanates and potassium tetratitanate earlier, taking off potassium through pickling again handles and further thermal treatment, could generate POTASSIUM HEXATITANATE fiber, and adopt multistep processes to increase technical process, material consumption and cost of equipment undoubtedly, unfavorable to scale production.The inventor once delivered one piece of communication " development of potassium titanate crystal whisker " in 1992 in " progress in materials science " on the fifth phase, a kind of potassium titanate crystal whiskers preparation method is disclosed, to contain the Ti compound is the Ti source, sylvite is the potassium source, add suitable fusing assistant and catalyzer, synthetically grown under high temperature oxidation atmosphere generates whisker.The end relates to the variety type of any solubility promoter that adopts and catalyzer in the tube news, consumption and proportioning etc., and the adding of catalyzer certainly will increase production cost.
The object of the present invention is to provide a kind of method of making potassium titanate fiber more simply, it need not add catalyzer, can improve synthesis efficiency and whisker quality, reduces cost, and makes things convenient for the big batch continuous production.
The invention provides a kind of preparation method of potassium titanate crystal whisker, with titanium-containing compound and potassium-containing compound is raw material, and add fusing assistant, it comprises batch mixing, synthetic, hydrolysis, filtration and exsiccant step, and it is characterized in that: fusing assistant is one of base metal nitrate, vitriol, muriate or its combination; Raw material is 2～4: 1 (More's ratio) preparation by Ti: K, and the amount of fusing assistant is 20～40wt%, 900～1300 ℃ of synthesis temperatures, 30 minutes～4 hours time.
Described titanium-containing compound can be Rutile type Titanium Dioxide, anatase octahedrite, titanium dioxide, and potassium-containing compound can be potassium hydroxide, saltpetre, Repone K, salt of wormwood.
Adopting the method for the invention can generate diameter is that 1～5 μ m, length are the six potassium titanate (K of 20～80 μ m
2Ti
6O
13) whisker.Owing in the mixing of raw material, added the fusing assistant of suitable proportion, formed the uniform mixing of raw material and fusing assistant; The fusing assistant fusing point is lower, thereby greatly reduces the synthesis temperature of fiber growth; The flux melt forms the growth that the liquid phase space benefits potassium titanate fiber, helps to improve the whisker quality; The proportioning raw materials that the present invention adopts, helping step generation six potassium titanates (is K
2Ti
6O
13) fiber, than scorification, earlier synthetic unsettled two potassium titanates of the gentle cold crystallization method of quick cooling crystallization method and potassium tetratitanate, to take off potassium through pickling again and handle and further thermal treatment, the multistep processes that could generate POTASSIUM HEXATITANATE fiber seems superior.Below by embodiment in detail the present invention is described in detail.
Embodiment 1:
1. preparation of raw material: titanium-containing compound adopts anatase titanium dioxide breeze (TiO
2Account for more than 95%); Potassium-containing compound adopts Repone K (purity 96%), presses Ti/KMol than 2.5 prescriptions, adds fusing assistant 20wt.% sodium-chlor and mixes; 2. put into cabinet-type electric furnace and be heated to 1000 ℃, be incubated 2 hours, then furnace cooling; 3. burned material is put in to soak in the water of 10 times (weight ratios) and blends; 4. filter and remove moisture, dry in electric oven; Resultant white needles thing is crystal whisker of hexa potassium titanate through X-ray diffraction analysis and scanning electron microscopic observation.Diameter is 1～4 μ m, and length is at 20～50 μ m, and quality is even, structural integrity.
Embodiment 2:
1. preparation of raw material: titanium-containing compound adopts rutile-type ilmenite powder (TiO
2Account for more than 95%); Potassium-containing compound adopts saltpetre (purity 98%), presses Ti: K Mol adds fusing assistant 30wt.% sodium-chlor, uniform mixing than 3 prescriptions; 2. raw materials mixed is placed in the punching block extrusion forming; 3. moulding sample piece is put into cabinet-type electric furnace and is heated to 1100 ℃, is incubated one hour, then furnace cooling; 4. burned material is put in to soak in the water of 10 times (weight ratios) and blends; 5. filter and remove moisture, dry in electric oven; Resultant white needles thing is crystal whisker of hexa potassium titanate through X-ray diffraction analysis and scanning electron microscopic observation.Diameter is 0.5～2 μ m, and length is at 20～50 μ m, and quality is even, structural integrity.
Embodiment 3:
1. preparation of raw material: titanium-containing compound adopts titanium oxide powder (TiO
2Account for more than 95%); Potassium-containing compound adopts saltpetre (purity 98%), presses Ti/K Mol than 3.8 prescriptions, adds fusing assistant 40wt.% sodium sulfate and mixes;
2. compound is put into cabinet-type electric furnace and be heated to 1300 ℃, be incubated 30 minutes, then furnace cooling; 3. burned material is put in to soak in the water of 10 times (weight ratios) and blends; 5. filter and remove moisture, dry in electric oven; Resultant white needles thing is crystal whisker of hexa potassium titanate through X-ray diffraction analysis and scanning electron microscopic observation.Diameter is 0.5～2 μ m, and length is at 20～60 μ m, and quality is even, structural integrity.
Embodiment 4 (comparative example):
The quick cooling crystallization method
[4.5]: 1. preparation of raw material: titanium-containing compound adopts rutile-type breeze (TiO
2Account for more than 95%); Potassium-containing compound adopts salt of wormwood (purity 99%), presses TiO
2/ K
2O Mol is than 3.0 prescriptions; Uniform mixing; 2. heating and melting: raw material is placed in the crucible, puts into cabinet-type electric furnace and is heated to 1300 ℃, is incubated 30 minutes; 3. quick cooling crystallization: with two roller foliation methods (roller footpath 80mm, two roller spacing 0.3mm, roller speed 90rpm) the foil-like solid; 4. pulverize: the foil-like solid is ground into granularity 0.5～10 μ m; 5. taking off potassium handles: crushed material is put in the water of 50 times (weight ratios) or the acetic acid soaks a few hours; 6. thermal treatment: filter and remove moisture, in electric oven,, be incubated 10～24 hours at 1000 ℃ then in dry; 7. separate fibre: in the article after thermal treatment, add 10 times of water, stirred 15 minutes; 8. dehydrate: get the white needles thing,, be potassium tetratitanate and six potassium titanate blend fiber through X-ray diffraction analysis and scanning electron microscopic observation.Diameter is 0.5～2 μ m, and length is in 10～30 μ m, inferior quality.
Compared and can obviously be found out by embodiment and comparative example: method preparation technology of the present invention simplifies greatly, saved pulverizing, taken off multiple working procedures such as potassium and thermal treatment, and synthesis reaction temperature reduces greatly, and resulting fiber is longer, and quality is better.Application result shows: the prepared whisker of the inventive method has performances such as lightweight, high-strength, fire-resistant, heat insulation and abrasion resisting, can be used as the heat resisting coating additive, automobile brake sheet also is widely used in polymer matrix composites as strengthening constituent element, is the best product that replaces asbestos.By preparation technology provided by the invention, method is easy, with low cost, and non-environmental-pollution is applicable to industrial-scale production.
Pertinent literature: [1] " ceramic industry association will ", 83, (1975) p.305～311[2] " ceramic industry association will ", 88, (1980) p.84～91[3] " ceramic industry association will ", 90, (1982) p.19～23[4] JP 63-79799 [5] JP 63-79800[6] " ceramic industry association will ", 91, (1983) p.189
Claims (2)
1. the preparation method of a potassium titanate crystal whisker, with titanium-containing compound and potassium-containing compound is raw material, and add fusing assistant, and it comprises batch mixing, synthetic, hydrolysis, filtration and exsiccant step, it is characterized in that: fusing assistant is one of base metal nitrate, vitriol, muriate or its combination; Raw material is 2～4: 1 (More's ratio) preparation by Ti: K, and the amount of fusing assistant is 20～40wt%, 900～1300 ℃ of synthesis temperatures, 30 minutes～4 hours time.
2. by the described Preparation of Whiskers method of claim 1, it is characterized in that: raw material compacting to mixing before synthetic.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93111038A CN1035443C (en) | 1993-04-10 | 1993-04-10 | Potassium titanate crystal whiskers preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93111038A CN1035443C (en) | 1993-04-10 | 1993-04-10 | Potassium titanate crystal whiskers preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1093760A CN1093760A (en) | 1994-10-19 |
| CN1035443C true CN1035443C (en) | 1997-07-16 |
Family
ID=4988845
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN93111038A Expired - Fee Related CN1035443C (en) | 1993-04-10 | 1993-04-10 | Potassium titanate crystal whiskers preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1035443C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348275C (en) * | 2005-05-18 | 2007-11-14 | 河北工业大学 | Method for preparing surface microporous titanium of titanium-based biological medical material |
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|---|---|---|---|---|
| CN1074391C (en) * | 1997-06-12 | 2001-11-07 | 中国科学院固体物理研究所 | fibrous nanometer potasium titanate and its preparing method |
| CN101144186B (en) * | 2006-09-12 | 2011-11-23 | 江西隆亨新材料有限公司 | Method for synthesizing potassium hexatitanate crystal whisker |
| CN101250751B (en) * | 2007-11-30 | 2010-06-09 | 江苏大学 | A kind of method for preparing potassium hexatitanate whisker |
| CN101962808B (en) * | 2010-06-17 | 2012-05-23 | 马玉馨 | High-efficiency and energy-saving potassium titanate whisker preparation method |
| CN102070188A (en) * | 2010-12-09 | 2011-05-25 | 江南大学 | Method for preparing difficult-to-harden potassium titanate with low hygroscopicity and high bulk density |
| CN102677173A (en) * | 2012-05-22 | 2012-09-19 | 中国科学院青海盐湖研究所 | Preparation method of lead titanate whiskers |
| CN102787359B (en) * | 2012-09-03 | 2015-04-15 | 中国科学院青海盐湖研究所 | Preparation method for calcium titanate whiskers |
| CN102849790B (en) * | 2012-09-27 | 2014-10-01 | 攀枝花学院 | Preparation method of columnar potassium hexatitanate |
| CN104005080A (en) * | 2014-05-30 | 2014-08-27 | 中国科学院过程工程研究所 | Preparation method of titanium containing crystal whisker |
| CN104894636B (en) * | 2015-04-29 | 2017-10-27 | 华东理工大学 | The preparation method of eight potassium titanate crystal whiskers |
| CN105734670B (en) * | 2016-04-13 | 2017-11-14 | 唐山晶须复合材料制造有限公司 | A kind of synthetic method of potassium hexatitanate cylindrulite |
| CN108315822B (en) * | 2018-02-10 | 2020-12-18 | 罗旭 | Epoxy-driven one-step preparation of potassium hexatitanate whiskers and its photocatalytic application |
| CN110697767B (en) * | 2019-11-07 | 2022-08-05 | 河钢股份有限公司承德分公司 | Method for preparing alkali metal fluorotitanate by using alkali metal titanate |
| CN111116156B (en) * | 2019-12-19 | 2022-01-25 | 江苏盐砼新材料科技有限公司 | Low-damage high-strength aerated concrete block and preparation method thereof |
| CN112030221A (en) * | 2020-08-06 | 2020-12-04 | 西安近代化学研究所 | High length-diameter ratio K2Ti6O13Preparation method of whisker |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0283300A (en) * | 1988-09-21 | 1990-03-23 | Toho Titanium Co Ltd | Heat treatment of potassium titanate whisker |
-
1993
- 1993-04-10 CN CN93111038A patent/CN1035443C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0283300A (en) * | 1988-09-21 | 1990-03-23 | Toho Titanium Co Ltd | Heat treatment of potassium titanate whisker |
Non-Patent Citations (1)
| Title |
|---|
| 材料科学进展92.V6.NO.5 1992.10.1 隗学礼；钛酸钾晶须的研制 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348275C (en) * | 2005-05-18 | 2007-11-14 | 河北工业大学 | Method for preparing surface microporous titanium of titanium-based biological medical material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1093760A (en) | 1994-10-19 |
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