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seems as if the adherent bacterial plaque had a similar composition, regardless of

material [3-198]. Sordyl et al. [3-203] collected bacterial samples from the superior

aspect of implants after bar and abutment were removed. They found that the plaque

specimens contained a predominantly gram-positive microflora, although gram-neg-

ative species were present in low numbers [3-203]. Balkin et al. [3-204] examined

the peri-implant microboita of human mandubular subperosteal dental implants. The

study established that gram-positive facultative Streptococcus and Actinomyces spp.

are characteristic of subperiosteal implants with long-term clinical stability. Al Saleh

et al. [3-205] studied the amount of plaque formation that occurs on CpTi, Ti-6Al-

4V, gold, and enamel by using an artificial mouth system. S. mutans and S. sanguis

were used as the test bacteria. The metals and control teeth were exposed to S.

mutans for 2 days and S. sanguis for 3 days. It was reported that (i) a mean S. mutans

coverage was 44% on the enamel, 98.5% on the gold, 91.8% on the CpTi, and 91.2%

on the Ti-6Al-4V alloy, (ii) there was a statistically significant difference between

enamel and the three metals, (iii) the mean of S. sanguis coverage was as follows:

48.3% on enamel, 50.4% on gold, 13% on CpTi, and 27.3% on Ti-6Al-4V alloy, and

(iv) CpTi harbored less S. sanguis than enamel and gold, whereas enamel harbored

less S. mutans than gold, CpTi and Ti-6Al-4V alloy [3-205].

While there is considerable information about bacteria adhesion on enamel, lit-

tle is known about the mechanism of bacterial interactions with implant materials

in the oral cavity [3-194]. It was found that in edentulous mouths, the presence of

gram-positive cocci around implants was significantly greater than that of other

bacteria [3-206]. In partially edentulous, healthy or diseased mouths, implants and

teeth harbored the same type of bacteria [3-207, 3-208]. No significant differences

were found between the subgingival flora of teeth and titanium implants in an

in vivo study [3-209] of a periodontally healthy mouth. Microbial plaque accumu-

lation surrounding dental implants may develop into peri-implantitis or peri-

impantoclasia, which is defined as inflammation or infection around an implant,

with accompanying bone loss [3-210]. Peri-implant disease can be as destructive

as periodontal disease, and adequate diagnosis and timely treatment are essential.

The microflora around successful implants is similar to healthy sulci, while that

associated with failing implants is similar to periodontally diseased sites. Implant

microflora is similar to the tooth microflora in the partially edentulous mouth. The

microflora of implants in partially edentulous mouths differs from that in edentu-

lous mouths. This seems to indicate a bacterial reservoir around the teeth and the

possibility of reinfection of the implant sulcus by periodontal pathogens [3-211].

It is, therefore, important to maintain plaque-free surfaces on both supra- and sub-

gingival portions of dental implants to prevent pre-implantitis. There are at least

two methods of inhibiting the formation of microbial plaque. The first method is

to inhibit the initial adhesion of oral bacteria. The second method is to inhibit the

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colonization of oral bacteria, which involves surface antibacterial activity.

Yoshinari et al. [3-212] studied the antibacterial effect of surface modifications to

Ti on P. gingivalis and A. actinomycetemcomitans. Surface modifications with the

dry process included (1) ion implantation (Ca

⫹

, N

⫹

, F

⫹

), (2) oxidation (anodic

oxidation, titania spraying), (3) ion plating (TiN, alumina), and (4) ion beam mix-

ing (Ag, Sn, Zn, Pt) with Ar

⫹

on CpTi plates. It was found that (i) F

⫹

-implanted

specimens significantly inhibited the growth of both P. gingivalis and A. actino-

mycetemcomitans than the untreated Ti, (ii) the other surface-modified specimens

did not exhibit effective antibacterial activity against both bacteria, and (iii) no

release of fluoride ions were detected from F

⫹

-implanted specimens under disso-

lution tests. It was thus indicated that surface modifications by means of a dry

process are useful in providing antibacterial activity of oral bacteria to Ti implants

exposed to the oral cavity [3-212].

Both anaerobic and aerobic bacteria can participate in the process of microbi-

ology-related corrosion. Sulfate-reducing bacteria are most prevalent under

anaerobic conditions. Lekholm et al. found that the microbial species around sta-

ble versus failing implants are similar to the patterns observed around healthy

versus periodontally involved teeth [3-213]. Quirynen et al. found no significant

differences in the bacterial morphotypes between implants and natural teeth in

partially edentulous patients (with implants and teeth in the same jaw). The per-

centages of coccoid cells, motile rods, spirochetes, and other bacteria were 65.8,

2.3, 2.1 and 29.8% for implants and 55.6, 4.9, 3.6, and 34.9% for teeth, respec-

tively. The results suggested that teeth may serve as a reservoir for the bacterial

colonization of Ti implants in the same mouth [3-207].

There exist several in vitro MIC-related corrosion tests. In an in vitro study using

Staphylococcus epidermidis, a simple-producing strain and its isogenic slime-neg-

ative mutant, it was found that (i) both strains adhere to CpTi discs with signifi-

cantly higher colony counts for the slime-producing strain, (ii) the colony count was

dependent on temperature, time, and stain, and (iii) slime production is important

for adherence and subsequent accumulation of S. epidermidis onto CpTi discs in

vitro [3-214]. Drake et al. [3-215] prepared CpTi surfaces by pre-treating (SiC pol-

ished, sand-blasted, 30% NHO

passivated), followed by exposing them to UV ster-

ilization, steam autoclaving at 121

C, ethylene gas treatment at 55

C, and plasma

cleaning in argon gas. These surface-modified CpTi were investigated in terms of

wettability, roughness, mode of sterilization, and the ability of the oral bacterium S.

sanguis to colonize. It was concluded that (i) Ti samples that exhibited rough or

hydrophobic (low wettability) surfaces, along with all autoclaved surfaces, were

preferentially colonized, (ii) Ti surfaces that had been repeatedly autoclaved were

colonized with the levels of bacteria 3 to 4 orders of magnitude higher than other

modes of sterilization, and (iii) this may have implications relative to the commonly

Chemical and Electrochemical Reactions 59

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used method of autoclaving titanium implants, which may ultimately enhance bac-

terial biofilm formation on these surfaces [3-215].

Bacterial reaction on teeth is different from that on titanium materials. Gibbons

and Van Houte [3-197] noted that the interaction of host flora with teeth involves

a highly selective process related to specific interactions between tooth-bound

salivary pellicles and bacterial surface adhesions. The ion distribution and charge

character of titanium should be different from enamel. Therefore, salivary pelli-

cle formation at each of these surfaces may in turn be different. It was found that

(i) using an in vitro adherence model significantly lowered numbers of A. visco-

sus bound to the salivary-treated Ti surface were found when compared to that of

the similarly treated enamel, (ii) the binding of S. sanguis to Ti or enamel did not

vary significantly, (iii) a comparison of the percentage of cells bound to the tita-

nium surface revealed that S. sanguis cells attached in significantly higher num-

bers when compared to the A. viscosus cells, and (iv) formation of salivary

protein pellicles on Ti may be quite different from that of enamel. It was further

speculated that the changes seen in the pellicle formation are the result of an

alteration in the rate of pellicle formation on Ti or the weakening of interactions

of the salivary proteins with the surface, as a result of the lowered surface free

energy [3-196], supporting observations by Fujioka-Hirai et al. [3-195].

Chang et al. [3-216] investigated electrochemical behaviors of CpTi, Ti-6Al-4V,

NiTi, Co-Cr-Mo, 316L stainless steel, 17-4 PH stainless steel, and Ni-Cr in (1)

sterilized Ringer’s solution, (2) S. mutans mixed with sterilized Ringer’s solution,

(3) sterilized tryptic soy broth, and (4) byproduct of S. mutans mixed with steril-

ized tryptic soy broth. It was concluded that (i) among the four electrolytes, the

byproduct mixed with sterilized trypic soy broth was the most corrosive media,

leading to an increase in I

CORR

and reduction in E

CORR

, (ii) CpTi, Co-Cr-Mo, and

stainless steel increased their I

CORR

significantly, but Ti-6Al-4V and NiTi did not

show remarkable increase in I

CORR

[3-216].

Koh [3-164] studied effect of surface area ratios on bacteria galvanic corro-

sion of commercially pure titanium coupled with other dental alloys. CpTi was

coupled with a more noble metal (type IV dental gold alloy) and a less noble

metal (Ni-Cr alloy) with different surface area ratios (ranging from 4:0 to 0:4

⫺ in other words, 4:0 uncouple indicates that entire surface area of a noble metal

was masked, while 0:4 uncouple indicates that only CpTi surface was masked,

and area ratios between 4:0 and 0:4 indicate that both surfaces were partially

masked to produce different surface areas). Galvanic couples were then electro-

chemically tested in bacteria culture media and culture media containing bacte-

ria byproducts. It was found that I

CORR

(and hence, corrosion rate) profiles as a

function of surface area ratio showed a straight-line trend (meaning surface area

ratio independence) for Ti/Au couples, whereas the representative curve for the

60 Bioscience and Bioengineering of Titanium Materials

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Ti/Ni-Cr alloy was bowl shaped. The latter curve indicates further higher corro-

sion rates at both ends (larger area of either CpTi or Ni-Cr), meaning that low-

est corrosion rate was exhibited at the bottom of bowl (at equal surface area

ratio) [3-164], supporting results obtained by Al-Ali et al. [3-165] and Garcia

and Oshida [3-169].

3.7. REACTION WITH HYDROGEN

It is generally agreed that the solubility of hydrogen in -phase titanium and tita-

nium alloys is quite low, namely on the order of 20⫺2000 ppm at room tempera-

ture [3-217]. However, severe problem can arise when Ti-based alloys pick up

large amounts of hydrogen, especially at elevated temperatures [3-218⫺3-222].

The strong stabilizing effect of hydrogen on the -phase field results in a decrease

of the  (HCP crystalline structure) →  (BCC crystalline structure) transforma-

tion temperature from 885

C to a eutectoid temperature of 300

C [3-218].

Hydrogen absorption from the surrounding environment leads to degradation of

the mechanical properties of the material [3-223]. This phenomenon has been

referred to as hydrogen embrittlement over the past years. Hydrogen absorption

often becomes a problem for high-strength steels even in air [3-224], and it also

occurs for Ti in methanol solutions contaning hydrochloric acid [3-225⫺3-229].

Hydrogen damage of Ti and Ti-based alloys is manifested as a loss of ductility

(embrittlement) and/or reduction in the stress-intensity threshold for crack propa-

gation [3-217]. CpTi is very resistant to hydrogen embrittlement, but it becomes

susceptible to hydrogen embrittlement under an existence of notch, at low tem-

perature, high strain rates, or large grain sizes [3-230]. Eventually, all of these

thermal and mechanical situations make the material more brittle in nature. For 

and near  Ti materials, it is believed that such hydrogen embrittlement occurs due

to precipitation of brittle hydride phases [3-231]. For ⫹ phase alloys, when a

significant amount of  phase is present, hydrogen can be preferentially trans-

ported with the  lattice, and will react with  phase at / boundaries. Under this

condition, degradation will generally become severe [3-232]. For  alloys, hydro-

gen embrittlement was observed to occur in the Ti-Mo-Nb-Al [3-233], Ti-V-Cr-

Al-Sn [3-234], and Ti-V-Fe-Al alloys [3-235], due to -hydride phase formation,

which is brittle at low temperatures [3-217].

It was confirmed that a shear crack initiated at the root of the thread and prop-

agated into the inner section of the screw in the dental implant systems. Gas chro-

matography revealed that the retrieved screw and absorbed a higher amount of

hydrogen than the as-used CpTi sample. It was then suggested that CpTi in a bio-

logical environment absorbs hydrogen, and that this may be the reason for delayed

fracture of Ti implants [3-224]. Such absorbed hydrogen might have two different

Chemical and Electrochemical Reactions 61

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sources. The first source of hydrogen is the internal hydrogen that is already pres-

ent in the material, either in solution or as hydrides. The second source is external

hydrogen, which is produced through the interaction between titanium and hydro-

gen or hydrogen producing environments (including cathodic reaction during the

corrosion reaction) during service. It is generally assumed that hydrogen from the

environment is taken up by the titanium, thereby becoming internal hydrogen.

Thus, the two effects are obviously very similar. As an alloying element in tita-

nium, hydrogen provides very little increase in strength but can seriously impair

both ductility and toughness [3-236⫺3-238].

There are some processes by which hydrogen could develop, and possibly be

absorbed, under passive conditions: direct absorption of hydrogen produced by water

hydrolysis and absorption of atomic hydrogen produced by the corrosion processes

to produce an oxide. Under anodic conditions, when passive corrosion prevails, the

corrosion potential for passive titanium must rise at a value at which water reduction

can cause titanium to oxidize, Ti ⫹ 2H

O →TiO

⫹ 2H

. Since Ti hydrides are ther-

modynamically stable at these potentials, the passive film can only be considered as

a transport barrier, and not an absolute barrier. The rate of hydrogen absorption will

be controlled by the rate of corrosion reaction, which dictates the rate of production

of absorbable hydrogen. Since TiO

is extremely insoluble, the corrosion reaction

will be effectively limited to an oxide film growth reaction [3-239]. Titanium corro-

sion processes are often accompanied with hydrogen production, introducing the

possibility of the absorption of hydrogen into the material. Crevice corrosion, once

initiated, is supported by both the reduction of oxygen on passive surfaces external

to the crevice and the reduction of protons (Ti ⫹ 4H

⫹

→ Ti

4⫹

⫹ 2H

) inside the

crevice, leading to the absorption of atomic hydrogen in sufficient quantities to pro-

duce extensive hydride formation. For passive non-creviced or inert crevice condi-

tions, corrosion could be sustained by reaction with water under neutral conditions

(Ti ⫹ 2H

O → TiO

⫹ 2H

), and should proceed at an extremely slow rate. In the

first step to possible failure by hydrogen-induced cracking, the hydrogen generated

must pass through the TiO

film before absorption into the underlying titanium alloy.

For absorption to proceed, redox transformation (Ti

4⫹

→ Ti

3⫹

) in the oxide film is

necessary. This requires significant cathodic polarization of the metal, generally

achievable by galvanic coupling to active materials (such as carbon steel), or appli-

cation of cathodic protection potential [3-240].

Ogawa et al. [3-223] conducted immersion tests on a beta Ti alloy (77.8Ti-

11.3Mo-6.6Zr-4.3Sn) under sustained tensile load (0⫺900 MPa) for various peri-

ods at room temperature, in 0.2 and 2.0% APF (2% NaF⫹1.7% H

Hydrogen absorption behavior of in acid fluoride solution has been analyzed by

hydrogen thermal desorption. It was reported that (i) in the case of an immersion

time of 60 h, the amount of absorbed hydrogen exceeded 10,000 ppm, while the

62 Bioscience and Bioengineering of Titanium Materials

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amount of hydrogen absorbed in the 0.2% APF solution was several times smaller

than that in 2% solution, (ii) for immersion in 0.2% APF, hydrogen absorption

saturated after 48 h, and (iii) during the later stage of immersion, the amount of

absorbed hydrogen markedly increased under higher applied stress, although the

applied stress did not enhance hydrogen absorption during the early stage of

immersion. These results of hydrogen absorption behavior are consistent with the

delayed fracture characteristics of the beta Ti alloy [3-223].

Lane et al. [3-241] tested various Ti alloy cantilever beam specimens, and

reported that seawater embrittlement behavior is related to aluminum content,

aging in the range of 480⫺700

C, and the presence of isomorphous beta stabiliz-

ers (Mo, V, Co). Test results indicate that (i) seawater embrittlement is an environ-

ment-dependent brittleness triggered by an aqueous corrodent, (ii) seawater

sensitive Ti alloys include CpTi, Ti-7Al-2Nb-1Ta, Ti-7Al-3Nb, Ti-6Al-2.5Sn, and

Ti-6Al-3Nb-2Sn, whereas sea water insensitive Ti alloys include Ti-7Al-2.5Mo,

Ti-6Al-2Sn-1Mo-1V, Ti-6.5Al-5Zr-1V, Ti-6Al-4V, and Ti-6Al-2Sn-1Mo-3V, and

(iii) in order to reduce embrittlement, it is recommended to lower Al content, and

to add elements (Mo or V) that suppress the formation of coherent Ti

Al [3-241].

Superelastic NiTi wire is widely used in orthodontic clinics, but delayed fracture

in the oral cavity has been observed. Because hydrogen embrittlement is known to

cause damage to Ti alloy systems, Yokoyama et al. [3-242] treated orthodontic wires

cathodically in 0.9% NaCl solution for charging hydrogen, followed by conducting

tensile tests and fractographic observations. It was reported that (i) the strength of

the Co-Cr alloy and stainless steel used in orthodontic mechanotreatment was not

affected by the hydrogen charging; however, NiTi wire showed significant decreases

in its strength, and (ii) the fractured surface of the alloy with severe hydrogen charg-

ing exhibited dimple patterns similar to those in the alloys from patients. In view of

the galvanic current in the mouth, the fracture of the NiTi alloy might be attributed

to the degradation of the mechanical properties due to hydrogen absorption [3-242].

Hydrogen-induced embrittlement of NiTi was also found when it was tested in acidic

solutions, and fluoride-containing solutions such as APF [3-243, 3-244]. However, it

was suggested that the work-hardening NiTi alloy was less sensitive to hydrogen

embrittlement compared with NiTi superelastic alloy [3-226].

Titanium reaction with hydrogen is not necessarily a useless phenomenon. The

formation of titanium hydrides can provide an engineering advantage. It is well

known that titanium is one of the most promising materials for hydrogen storage

due to a stable formation of non-stoichiometric titanium hydrides (, , or  type)

over the composition range from TiH

1.53

to TiH

1.99

[3-225].

Finally, the unique reaction of titanium with hydrogen can be used favorably for

the grain refining, which has a sequence of hydrogen absorption → heat treatment

and working → de-hydrogen treatment. For example, Ti-3Al-2.5Sn containing 0.5

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mass% of hydrogen was heated at 780

C and solid-solution treated, followed by

water-quenched to have martensitic phase. The alloy was further subjected to hot-

rolling in the ⫹ dual structure, followed by heating at 600

C in vacuum to de-

hydrogen treatment [3-229]. Such treated Ti-3Al-2.5Sn shows uniaxial

microstructrue with the grain size in a range from 0.5 to 1 m, which is suitable

for the superelastic forming.

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