CN100496979C - Substrate for ink jet head, ink jet head using the same, and manufacturing method thereof - Google Patents
Substrate for ink jet head, ink jet head using the same, and manufacturing method thereof Download PDFInfo
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- CN100496979C CN100496979C CNB2003801075185A CN200380107518A CN100496979C CN 100496979 C CN100496979 C CN 100496979C CN B2003801075185 A CNB2003801075185 A CN B2003801075185A CN 200380107518 A CN200380107518 A CN 200380107518A CN 100496979 C CN100496979 C CN 100496979C
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Abstract
The present invention provides a substrate for ink jet including a heating resistor generating thermal energy for discharging an ink from an ink discharge port and an upper protective layer which is formed above the heating resistor and has a contacting surface with the ink. Furthermore, the upper protective layer is made of an amorphous alloy consisting of Ta and Cr in which the content of Ta is more than that of Cr. This constitution allows for the substrate excellent in cavitation resistance and corrosion resistance, and capable of high durability while having similar discharge performance to that of a conventional protective layer made of a Ta film. The present invention further provides an ink jet head comprising the above-mentioned substrate, and a manufacturing method thereof.
Description
Technical field
The present invention relates to be ejected into the used substrate of ink gun of the recording medium that comprises paper, plastic sheet, cloth, article etc. such as the functional liquid of printing ink; Use the ink gun and the manufacture method thereof of this substrate.
Background technology
For a kind of conventional structure that is used for the ink gun of ink mist recording, can adopt a kind of like this structure, a plurality of outlets, the ink flow passage that links to each other with these outlets and a plurality of electrothermal conversioning element that can produce the heat energy that is used for ink-jet wherein are set.Each electrothermal conversioning element has heating resistor and for heating resistor provides the electrode of electric energy, and this electrothermal conversioning element scribbles insulation film to guarantee the insulation between each electrothermal conversioning element.Each ink flow passage links to each other with common liquid chamber at its place, end relative with the outlet of ink flow passage, and in common liquid chamber, is stored by the printing ink of supplying with as the ink box of printing ink storage container parts.The printing ink that supplies to public ink chamber leads to each ink flow passage so that printing ink forms meniscus near outlet.In this state, electrothermal conversioning element is selectively driven to produce heat energy, and then utilize the energy that produced fast to the printing ink heating and on the heat effect surface, produce bubble, so that under by the pressure that described state variation caused, discharge printing ink.
Therefore during the printing ink efflux time, the heat effect of ink gun partly is heated resistor heats and is exposed under the higher temperature, and simultaneously, heat effect is partly united and is subjected to because the foaming of printing ink and cavitation shock that contraction causes and the chemical action of printing ink.This chemical action of printing ink can be brought following phenomenon.Particularly, be included in look material in the printing ink, additive etc. and at high temperature be heated, thus they on molecular level, decompose and change into and be difficult to dissolved substances, described material physically is absorbed on the upper protective layer.This phenomenon is known as fouling (kogation).When the organic and inorganic substances that are difficult to dissolve were absorbed on the upper protective layer by this way, the heat conduction from the heating resistor to printing ink became inhomogeneous, and therefore, bubbling becomes unstable.
Up to now, the Ta film that can stand the chemical action of cavitation shock and printing ink largely has been formed to such an extent that have the thickness of 0.2 to 0.5 μ m, thereby can increase the service life and the reliability of ink gun.
With reference to Fig. 9, will make detailed description about the foaming of printing ink and the state that foaming stops to be caused in the heat effect part.
Curve among Fig. 9 (a) shows at driving voltage V
Op=1.3 * V
Th(V
ThExpression printing ink foaming threshold voltage), driving frequency is set to 6kHz and pulse width is set under the situation of 5 μ s, the moment when voltage is applied in heating resistor begins the surface temperature change in time of upper protective layer.In addition, curve (b) shows moment when voltage is applied in heating resistor in a similar manner begin to be shaped growth state of bubble.Shown in the curve (a), begin the rising of temperature from the moment that voltage is applied in, and observe the back (this is slightly to arrive upper protective layer evening owing to come from the heat of heating resistor) that the temperature rise peak value is in the predetermined pulse time slightly.Afterwards, mainly reduce owing to the thermal diffusion temperature.On the other hand, shown in curve (b), when the temperature when upper protective layer reaches about 300 ℃, beginning the growth of bubble, and reach maximum foaming afterwards, foaming stops.In actual ink gun, repeat aforesaid operations.By this way, along with the foaming of printing ink, the surface temperature of upper protective layer is elevated to for example about 600 ℃, and this explanation is carried out ink mist recording by the heat effect under the high temperature.
Therefore, require to have outstanding membrane property at aspects such as hear resistance, mechanical property, chemical stability, non-oxidizability, alkali resistances with the contacted upper protective layer of printing ink.As the material that is used in the upper protective layer aspect; except that the above-mentioned Ta film of mentioning, noble metal, high-melting-point transition metal, the alloy of these metals, nitride, boride, silicide or carbide, the non-crystalline silicon etc. of these metals in addition known in the prior art.
For example, described in Japanese patent application laid-open publication number No.2001-105596, upper protective layer is formed on the heating resistor via insulating barrier, wherein upper protective layer is by composition formula Ta
αFe
βNi
γCr
δThe amorphous alloy of expression make (wherein satisfy 10at.%≤α≤30at.%, alpha+beta〉80at.%, α＜β, δ γ and alpha+beta+δ+γ=100at.%), and the contact surface of itself and printing ink comprises the oxide of component substances, has therefore proposed a kind of more reliable record head of long life that has.
Yet, in recent years, in higher-quality document image and the ink jet recording device such as more high performance increases in demand such as high-speed records, and, require the ink performance that strengthens in order to satisfy these demands.For example, in order to obtain that the high-quality document image has proposed the requirement of improved painted characteristic and weather resistance and in order to obtain the requirement that high-speed record has proposed to prevent bleeding (obscuring between the different colours printing ink).Therefore, made the trial of in printing ink, adding various compositions.About the kind of printing ink, except that black, yellow, magenta and cyan, to have developed by reducing the light color inks that concentration etc. obtains, this has brought the variation of printing ink.In some cases, a kind of like this phenomenon has appearred, that is, or even think traditionally can be stably as the Ta film of upper protective layer owing to the thermal chemical reaction with printing ink causes corrosion.Use therein to comprise such as divalent metal salt such as calcium and magnesium or constitute under the situation of printing ink of composition of chelate, can occur above-mentioned phenomenon more significantly.
In order further to quicken ink mist recording, require by than shorter in the past pulsed drive (that is, driving) by the driving frequency that increases.In described shorter pulsed drive, owing to the program that in the heat effect part of ink gun, repeats at short notice to heat, bubble, bubble and stop and cooling off, therefore to compare with traditional ink gun, this heat effect part stands bigger thermal stress at short notice.And printing ink will bubble and the cavitation shock of contraction concentrates on the upper protective layer because shorter pulsed drive will come from than the shorter in the past time, and therefore expectation exists in the upper protective layer that mechanical shock characteristic aspect is particularly splendid.
Though made various improvement; yet still found such problem; promptly; under the situation that has formed aforesaid upper protective layer with improved anti-ink corrosion performance; use certain printing ink can produce, thereby reduced discharging performance owing to fouling obviously is deposited on the product that causes on the heating part.
In addition, as the manufacture method of the substrate that is formed with above-mentioned upper protective layer that is used for ink-jet, use technology in many cases usually by dry etching.Yet in the situation that has formed the upper protective layer with improved anti-ink corrosion performance, although can keep high durability for a long time, indication becomes difficult by the technology of formations desired pattern such as etching etc.Fig. 8 A shows this situation to 8E.To as shown in the 8E, in the pattern of upper protective layer formed, it is etched that the normally used in many cases technology by dry etching can cause contacting the insulating protective layer of upper protective layer as Fig. 8 A.If as the etching selectivity that can guarantee fully in conventional substrate between insulating protective layer and the upper protective layer, but etching leaves the upper protective layer of insulating protective layer so.In fact, and upper protective layer between the over etching of boundary portion office can produce rank (among Fig. 8 E between A and the B).Since a kind of like this phenomenon, thus owing to causing the insulating protective layer of boundary portion office to become thinner, etching has than expecting the littler film thickness b of film thickness b, and this will cause the insufficient of its defencive function to apply.Therefore, must take etching gas into consideration and carry out the controlled condition that pattern forms afterwards according to an etching period acquisition etching upper protective layer for the etching speed of upper protective layer.Yet, found such problem, promptly; owing to upper protective layer may not etchedly stay; perhaps opposite, owing to cause the insulating protective layer can be etched owing to the inhomogeneities or the etching condition of device, thus the pattern that can not stably carry out upper protective layer forms.
Summary of the invention
An object of the present invention is to provide the ink gun with a kind of like this protective layer, described protective layer is outstanding aspect cavitation resistance and corrosion resistance, and has high durability, has the similar discharging performance of making to the Ta film of traditional protection layer simultaneously.
The ink gun that another object of the present invention provides a kind of substrate that is used to comprise a kind of like this ink gun of protective layer, comprise described substrate with and manufacture method; even used with the corresponding point of meticulous document image, with corresponding high-speed driving of high-speed record or various printing ink, described protective layer also has long service life.
Another object of the present invention provide a kind of be used for comprising produce be used for from the printing ink outlet discharge printing ink heat energy heating resistor and be located at above the heating resistor and have the contact surface that contacts with printing ink upper protective layer ink gun substrate, comprise described substrate ink gun with and manufacture method, described upper protective layer is made by the amorphous alloy that comprises Ta and Cr (wherein the content of Ta is greater than the content of Cr).
Description of drawings
Fig. 1 is partial cross section figure, shows the substrate that is used for the ink gun that the present invention is suitable for.
Fig. 2 A, 2B, 2C, 2D, 2E, 2F, 2G and 2H show the view that forms the method for injection component on the substrate that is used for the ink gun that is suitable in the present invention.
Fig. 3 shows the illustrative view of the film forming device of each layer that is used to form the substrate that is used for the ink gun that the present invention is suitable for.
Fig. 4 shows an illustrative view that constitutes example of the ink jet recording device that the ink gun that the present invention is suitable for is housed.
Fig. 5 A, 5B, 5C and 5D show in upper protective layer burnt deposit with and the illustrative view of the state that separates.
Fig. 6 A, 6B and 6C show the illustrative view in the cross section of observed heating element heater in discharging durability test.
Fig. 7 shows the chart with respect to the etching speed of Ta content.
Fig. 8 A, 8B, 8C, 8D and 8E show the view how upper protective layer stands dry etching.
Fig. 9 shows the chart in temperature that applies voltage upper back protective layer and the variation in the bubblement.
The specific embodiment
Fig. 1 is illustrative partial cross section figure, shows the substrate that is used for the ink gun that the present invention is suitable for.
In Fig. 1, Reference numeral 101 expression silicon substrates, the heat accumulation layer that Reference numeral 102 expressions are made by heat oxide film.The interlayer film that Reference numeral 103 expressions are made by SiO film, SiN film etc.; interlayer film 103 also has the function of gathering heat; Reference numeral 104 expression thermoresistance layers; Reference numeral 105 expressions are as the protective layer of being made by SiO film, SiN film etc. by the metal wiring layer of making such as metallic alloy such as Al, Al-Si and Al-Cu as wiring, Reference numeral 106 expressions, and protective layer 106 is also as insulating barrier.Reference numeral 107 expression is located at the upper protective layer on the protective layer 106, the chemistry and the physical impact of the heating that is used to protect electrothermal conversioning element not come from heating resistor.In addition, Reference numeral 108 expression heat effect parts, in this heat effect part 108, the heat that produces in the heat-resistant element of thermoresistance layer 104 acts on the printing ink.
Heat effect in the ink gun partly be owing to the heat that produces in the heating resistor be exposed under the high temperature and come from mainly that printing ink bubbles or bubble after the cavitation shock of bubble shrinkage or the part of the chemical action of printing ink.Therefore, this heat effect partly has the upper protective layer 107 of the chemical action that is used to protect electrothermal conversioning element not to be subjected to this cavitation shock or printing ink.Upper protective layer 107 stands dry etching by chlorine etc. after applying the mask of predetermined image or the resist of predetermined pattern (resist) stands wet etching by hydrofluoric acid, boric acid, hydrochloric acid etc. afterwards so that form pattern applying.Afterwards, on upper protective layer 107, use flow path to form element 109 and formed injection component with the outlet 110 that is used to discharge printing ink.
Fig. 2 A has wherein formed flow path and outlet to the method that 2H shows the injection component that is used to form ink gun on the upper protective layer 107 that forms pattern.
As shown in Fig. 2 A, under 400 ℃ temperature conditions, will have the SiO of about 2 μ m thickness by the CVD method
2Film 502 is formed on the lower surface of the substrate that is used for ink gun 501 (comprise silicon substrate 101, heat accumulation layer 102, interlayer film 103 and stand thermoresistance layer 104, metal wiring layer 105, insulating protective layer 106 and the upper protective layer 107 that predetermined pattern forms respectively).Here, Reference numeral 507 is corresponding to heat effect part 108.
As shown in Fig. 2 B, resist is applied to this SiO
2On the film 502 so that in exposure and after developing by dry etching or wet etching formation opening 511.This SiO after forming through hole 513 after a while
2Film 502 will will form from opening 511 as mask and through hole 513.For example, under the situation of dry etching, use CF
4Carry out SiO as etching gas by reactive ion etching
2The etching of film 502, and under the situation of wet etching, use the hydrofluoric acid that contains buffer to carry out SiO
2The etching of film 502.
Next, as shown in Fig. 2 C, be formed on the upper surface side of substrate at PSG (phosphosilicate glass) film 503 that will have about 20 μ m thickness by the CVD method under 350 ℃ the temperature conditions.
Next, as shown in Fig. 2 D, psg film 503 is processed to form predetermined flow path pattern.Here, preferably use resist to process psg film, because this can not damage the SiO on the lower surface by dry etching
2Film 502.
Next, as shown in Fig. 2 E, the silicon nitride film 504 that will have about 5 μ m thickness by the CVD method under 400 ℃ temperature conditions is formed in the flow path pattern on the formed psg film 503.At this moment, also be filled silicon nitride film in the opening 502.
Here, because the film thickness of formed silicon nitride film defines the gap that the film thickness of the thickness of outlet and the previous psg film that forms defines ink flow path, thereby the printing ink that has influenced ink jet is significantly discharged characteristic, and determines the film thickness of silicon nitride film and psg film according to desired characteristic.
Next, as shown in Fig. 2 F, use the SiO that before has been shaped
2 Film 502 is formed on the silicon substrate 501 through hole 513 to be used as ink supply port as mask.Although can use any formation method of through hole, with CF
4With oxygen be preferred as ICP (inductively coupled plasma) engraving method of etching gas, this is because it can Power Groud damages substrate and can form at low temperatures.
Next, as shown in Fig. 2 G, use silicon nitride film 504 to form outlet 514 by dry etching as resist.Use aspect anisotropic etching outstanding reactive ion etching as this formation method.
Next, as shown in Fig. 2 H, use the hydrofluoric acid that contains buffer to remove from outlet 514 with psg film 503 elutions and with it.
Afterwards, thus be formed on the surface of outlet by the waterproofing agent film that plasma polymerization will comprise Si and printing ink supply element (not shown) is attached on the bottom side of silicon substrate 501 and finishes ink gun.
Except that aforesaid being used for forming the dry method of flow path and outlet on the substrate, also can use following wet method to make ink gun.
As shown in Fig. 2 A; by spin coating method resist is coated in as the soluble solids layer and is used for ink gun 501 substrate of (comprise silicon substrate 101, heat accumulation layer 102, interlayer film 103 and stand thermoresistance layer 104, metal wiring layer 105, insulating protective layer 106 and the upper protective layer 107 that predetermined pattern forms respectively), described resist will become at last and be the printing ink flow path.The resist of being made by PMIPK (poly-methyl isopropenyl ketone, polymethylisopropheyl ketone) is configured as the shape of printing ink flow path as negative resist and by the use photolithography techniques with it.Subsequently, form the coating resin layer so that form flow path or outlet.Before forming this coating resin layer, can carry out the processing of silane coupling connection as required and wait to improve adhesion.Forming under the situation of flow path pattern, be coated with rete and can be applied to the substrate that is used for ink gun by the coating process that can from known coating process, choose.Afterwards, by using anisotropic etch method, blasting method, anisortopicpiston engraving method etc. to form and 513 corresponding printing ink liquid supply ports from the rear side that is used for ink gun.More particularly, use the chemical anisotropic silicon engraving method of tetramethyl azanol (TMAH), NaOH, KOH etc. to can be used for forming the printing ink liquid supply port.Carry out subsequently by far ultraviolet and expose fully, carry out afterwards and develop and drying to remove the soluble solids layer.
In any technology, the heat effect of ink gun part all be since the heat that produces in the heating resistor be exposed to high temperature under and mainly come from printing ink foaming or foaming after the cavitation shock of bubble shrinkage or the part of the chemical action of printing ink.Therefore, heat effect partly has the chemistry of the heating that is used to protect electrothermal conversioning element not come from heating resistor and the upper protective layer 107 of physical impact.Requirement can have at outstanding membrane properties in aspect such as thermal resistance, mechanical property, chemical stability, non-oxidizability, alkali resistances with the contacted upper protective layer 107 of printing ink.According to the present invention, be formed with the amorphous alloy that constitutes by Ta and Cr (wherein the content of Ta is greater than the content of Cr).Amorphous alloy involved in the present invention is meant the alloy with the amorphous structure that demonstrates no peak value, the existence of particular crystal plane (perhaps if any, having extremely low peak value) and broad diffraction pattern case wherein has been shown in crystal structure analysis by the X-ray diffraction method.
Suppose that the content of Cr is expressed as y in the amorphous alloy, so preferably satisfy 0at.%＜y≤30at.%, and, be more preferably and satisfy 0at.%＜y≤25at.%.
From 50nm to 500nm, select the film thickness of this upper protective layer 107 in the scope of (preferably from 100nm to 300nm).
And the membrane stress of this upper protective layer has compression at least and preferably is not more than 1.0 * 10
10Dyn/cm
2
Under the situation that has formed above-mentioned upper protective layer 107 with improved corrosion resistance, because high corrosion resistance makes that its surface is difficult to damage, thereby be easy to produce product owing to fouling, this has reduced the printing ink velocity of discharge or feasible injection itself is unstable.Can infer; the reason that has produced less amount fouling product in traditional protection layer 107 in the employed Ta film is that the mode with balance has produced small corrosion and fouling product in the Ta film, thereby and the surface of Ta film because small corrosion and scraped off restriction fouling product and be deposited.
Yet, aforesaid, added the SUS composition with the upper protective layer 107 that improves corrosion resistance in, when increasing the Ta composition when suppressing the deposition of fouling product, can not improve durability.Presumable is that this is that this has reduced the Cr composition that is considered to help durability because the increase of Ta composition has caused the minimizing of SUS composition.
By adding upper protective layer 107 amorphizations that chemically stable Cr makes that the present invention was suitable for to traditional Ta layer; and obviously reduced the point that has grain boundary of the starting point that can become corrosion reaction, improved corrosion resistance thereby compare with traditional Ta layer.
And because upper protective layer 107 that the present invention was suitable for has the composition of high Ta content, so slightly microcorrosion is with the deposition of inhibition fouling product on the surface of upper protective layer, and this can keep the discharging performance with traditional Ta layer same degree.
Here, to 5D, the difference between Ta layer that tradition uses and the TaCr film involved in the present invention is described with reference to Fig. 5 A.
Fig. 5 A show upper protective layer 107 be under the situation about making by traditional Ta layer upper protective layer 107 and with the interfacial illustrative figure of printing ink.By driving heating resistor fouling product 301 is deposited in the heat effect part.In addition, make the Ta of upper protective layer 107 constitute oxide-film 302 by the heat that produces during driving.The film thickness of this oxide-film increases along with the increase of the quantity of driving pulse, and finally is completed into oxide-film along film thickness direction.As shown in Fig. 5 B, the part of this oxide-film 302 and fouling product 301 are separated with upper protective layer 107 together.Therefore can think that by this way, the deposition that has suppressed fouling product 301 is to keep discharging performance and to reduce the film thickness of upper protective layer 107.
On the contrary, as shown in Fig. 5 C, compare with the oxide-film of traditional Ta layer, in the upper protective layer 107 that the present invention was suitable for, with the interface of printing ink in oxide-film 302 be formed on the metal level 303 as thin as a wafer.As shown in Fig. 5 D, this oxide-film 302 and the fouling product 301 that is deposited are separated to suppress the deposition of fouling product 301 with upper protective layer 107 together, and this can keep discharging performance.At this moment, compare with the oxide-film of traditional Ta layer, because oxide-film 302 is formed as thin as a wafer, so reducing on the film thickness of upper protective layer 107 be little, therefore compares with traditional Ta layer, can think and improve durability.
Therefore, make upper protective layer 107 amorphizations by adding Ta that chemically stable Cr has proper content simultaneously, this can improve corrosion resistance and keep discharging performance simultaneously.
And, because upper protective layer 107 has the composition of high Ta content, therefore compare with traditional Ta can with make by chlorine upper protective layer etching speed reduce suppress lessly.Therefore reduced the etching quantity of insulating protective layer and can keep reliability.
Can use radio frequency (RF) power supply or dc power supply to make usually by the upper protective layer 107 of various film formation method manufacturing by magnetron sputtering system.
Fig. 3 shows total figure of the sputtering equipment that is used to form upper protective layer.
In Fig. 3, two types the target that Reference numeral 4001 expressions are made of Ta target and Cr target.Reference numeral 4002 expression flat targets, Reference numeral 4011 expressions are used to control the power supply that film formed flashboard on the substrate, Reference numeral 4003 expression substrate holder, Reference numeral 4004 expression substrates, Reference numeral 4006 expressions and target 4001 are connected with substrate holder 4003.In addition, in Fig. 3, the external heater that Reference numeral 4008 expressions provide in the mode that forms the periphery wall of chamber 4009 around film.External heater 4008 is used to regulate the environment temperature that film forms chamber 4009.The interior heater 4005 that is used to control underlayer temperature is arranged on the rear surface of substrate holder 4003.Both carry out the temperature control of substrate 4004 preferably to use interior heater 4005 and external heater 4008.
Carrying out the film that uses Fig. 3 equipment as described as follows forms.At first, using exhaust pump 4007 that air is formed the chamber 4009 from film is evacuated to up to 1 * 10
-5To 1 * 10
-6Pa.Next, via the mass flow controller (not shown) argon gas being incorporated into film from gas introducing hole 4010 forms in the chamber 4009.At this moment, regulate interior heater 4005 and external heater 4008 to obtain target substrate temperature and environment temperature.Then, power is provided to target 4001 from power supply 4006, and carries out sputter and discharge so that form film on substrate 4004 when regulating flashboard 4011.
According to the present invention, two types target, that is, Ta target and Cr target can be used for by wherein supply the synchronous sputtering method formation of the binary film of power from two power supplys that are connected in respective target.In this case, can control the power that is fed to respective target independently.Perhaps, prepare the multiple alloys target that its composition has been regulated in advance, and every kind of alloys target had the film of desired constituents with formation by the while sputter by sputter or two kinds of alloys target or more kinds of alloys target independently.
In addition, aforesaid, when forming upper protective layer 107, substrate is heated to up to 100 ℃ to 300 ℃ to realize strong film adhesiveness.In addition, form film, can realize strong film adhesiveness by the aforesaid sputtering method that can form particle with big kinetic energy.
By making membrane stress have compression at least, and it is made as 1.0 * 10
10Dyn/cm
2Or lower, can realize strong film adhesiveness equally.Be incorporated into the flow velocity of the argon gas in the film forming device, the power that puts on target or substrate heating temperature by setting in each case and can regulate this membrane stress.
No matter the protective layer 106 that is located at below the upper protective layer 107 is that the upper protective layer 107 that thick or thin, involved in the present invention amorphous alloy film is made preferably all is applicable.
Fig. 4 shows the outline view of an example of the ink-jet apparatus that the present invention is suitable for.Incidentally, although the ink-jet apparatus shown in Fig. 4 is old-fashioned, the present invention who is applied to nearest ink-jet apparatus can bring more effect.
Record head 2200 is installed on the balladeur train 2120 that engages with the helicla flute 2121 of guide spiro rod 2104, and described guide spiro rod 2104 rotates with the reciprocal rotation of CD-ROM drive motor 2101 by driving force transmission gear 2102 and 2103.Record head 2200 moves back and forth with balladeur train 2120 along guide rail 2119 along direction of arrow a and b.The moving direction that the pressboard 2105 that is used for the record-paper P that supplies with by recording medium feeding mechanism (not shown) crosses balladeur train 2120 is pressed in pressing plate 2106 with record-paper.
Reference numeral 2107 and 2108 expressions are as the photoelectrical coupler of the original position checkout gear of the direction of rotation that is used to confirm the existence of this zone king-rod 2109 and switch CD-ROM drive motor 2101.The element of the cap member 2111 that is used to cover whole record head 2200 is supported in Reference numeral 2110 expression, and Reference numeral 2112 expressions are used for the aspirator of the inside of suction cover element 2111, recover by the suction of described aspirator 2112 via cover gab 2113 executive logging heads 2200.Reference numeral 2114 expression cleaning doctors, Reference numeral 2115 represent to make the moving meter that this scraper moves along fore-and-aft direction.These are supported by body supports plate 2116.It should be understood that as cleaning doctor known cleaning doctor and present embodiment are applicable to this equipment.
In addition, Reference numeral 2117 expression is used to begin to be used to aspirate the bar of the suction of recovery, described bar moves along with moving of the cam 2118 that engages with balladeur train 2120, thereby comes from the mobile control that is subjected to known transmitting device (such as the clutch conversion) of the driving force of CD-ROM drive motor 2102.Be used for sending signal to the sidepiece that record control unit (not shown) that the heating part that is located at record head 2200 or control said mechanism drive is disposed in the recording equipment main body.
As mentioned above the ink jet recording device 2100 of Gou Chenging when moving back and forth on the whole width that makes record head 2200 at record-paper P with respect to the record-paper P executive logging of supplying with by the recording medium feeding mechanism on pressing plate 2106, and because record head 2200 makes in the above described manner, therefore described equipment can be realized high accuracy, high-speed record.
Hereinafter, form example with reference to the film of upper protective layer and use the example of the ink gun of the upper protective layer of making by this alloy film etc. to describe the present invention in detail.Yet the present invention is not limited to described example.
Be formed on evaluation physics membrane property under the situation on the silicon wafer using the equipment shown in Fig. 3 will be used in amorphous alloy layer in the upper protective layer involved in the present invention 17 with the above-mentioned film method of formationing.
At first, heat oxide film is formed on the silicon single crystal wafer (substrate 4004), the film that described silicon single crystal wafer is set at the equipment shown in Fig. 3 forms on the substrate holder 4003 in the chamber 4009.Then, using exhaust pump 4007 that air is formed the chamber 4009 from film is evacuated to up to 8 * 10
-6Pa.Afterwards, argon gas being incorporated into film from gas introducing hole 4010 forms in the chamber 4009 so that set the condition that the film of the following stated forms chamber 4009 inside.
Underlayer temperature: 200 ℃
Film forms the gaseous environment temperature of chamber interior: 200 ℃
Film forms the gas pressure of chamber interior: 0.3Ppa
Then, select any one and such power that is fed to respective target of setting as shown in table 1 in Ta target or the Cr target at every turn, form example 1 to 6 so that obtain film.Formed the Ta film in film forms example 1, formed the TaCr film that formed crystallization in the example 2, form the TaCr film of amorphous structure in the example 3 to 6 at film at film, they have the film thickness of 20nm on the heat oxide film of silicon wafer.
In addition, use Ta target and Ta
18Fe
61Cr
15Ni
6Target and such power that is fed to respective target of setting as shown in table 1 form example 7 so that obtain the film of amorphous structure.And use Cr target and Ta
18Fe
61Cr
15Ni
6Target and such power that is fed to respective target of setting as shown in table 1 form example 8 so that obtain the film of amorphous structure.
The sample experience RBS (rutherford backscattering) of above-mentioned acquisition is so that carry out constituent analysis.Its result is shown in the table 1.
Next, in order to carry out structural analysis, carry out X-ray diffraction for the TaCr film that is formed on the upper protective layer on the silicon wafer as mentioned above and measure.As a result, Ta
89Cr
11Demonstrate clearly demarcated diffraction peak, and Ta
78Cr
22Do not demonstrate specific diffraction peak, this shows the transformation from the crystal structure to the amorphous structure.
Next, determine the membrane stress of each sample based on the substrate distortion amount before and after the film formation.As a result of, observe a kind of like this trend, that is, when the Cr composition was higher, membrane stress was changed into tensile stress from compression, and the film adhesion reduces.By making membrane stress have compression at least and being set is 1.0 * 10
10Dyn/cm
2Or lower, can obtain similar strong film adhesion.
(table 1)
(structure of upper protective layer and the relation between the fouling)
(example 1)
Discharge the analyzed sample substrate of characteristic as involved in the present invention about printing ink, can use silicon substrate or be embedded with the silicon substrate of drive IC.In the situation of silicon substrate, form the SiO of 1.8 μ m thickness by thermal oxidation process, sputtering method, CVD method etc.
2Heat accumulation layer 102 (with reference to Fig. 1), and under the situation of the silicon substrate that is embedded with drive IC, form SiO with similar manufacturing process
2 Heat accumulation layer 102.
Next, by sputtering method, CVD method etc. form 1.2 μ m thickness by SiO
2The interlayer dielectric of making 103.Afterwards, use the Ta-Si target by reactive sputtering form 50nm thick with composition formula Ta
40Si
21N
39The heating resistor 104 of expression.At this moment, underlayer temperature is 200 ℃.Formed the Al film that is used as metal line 105 with 200nm thickness.
Then, using the photolithography art to carry out forms pattern and has formed the heat effect part 108 of removing the 30 μ m * 30 μ m of Al film.Then, the insulator of making by the plasma CVD method SiN that 300nm is thick forms protective layer 106.Afterwards, the Ta that 230nm is thick under the condition of the formation of the film shown in the table 1 example 3
78Cr
22Form upper protective layer 107.Subsequently, be that upper protective layer 107 forms pattern is used for ink-jet with manufacturing substrate by dry etching.In this case, preferably use TaCr film in the example of describing after a while 7 to 15.
And, aforesaid, can replace dry etching by the wet etching that uses hydrofluoric acid and form pattern is used for ink gun with manufacturing substrate as upper protective layer 107.
Next, use is made ink gun by the substrate that is used for ink-jet of any one method manufacturing.Afterwards, use this ink gun evaluation that is installed on a kind of like this ink jet recording device shown in Fig. 4 to discharge characteristic.
In this test, under the driving frequency of 5kHz, apply and have 1 * 10 of the pulse width that is made as 1 μ sec
8Measure the velocity of discharge of each sample after the driving signal of pulse.At this moment, driving voltage V
OpBe V
Th* 1.15.In addition, use the available printing ink (trade mark: the BCI-3e-Bk that Canon Inc. produces) that is used for ink-jet printer on the market.V
ThExpression printing ink is at its foaming threshold voltage that is discharged from down.
In example 1, although applying 1 * 10
8Measure the velocity of discharge after the driving signal of pulse, do not influence obvious main reduction that printing ink is discharged characteristic but also can not observe.And, by after estimating, observing the surface of heating resistor, can confirm the small adhesion of fouling product.
(embodiment 2 and 3)
Use with example 1 similar methods and constitute TaCr film so that estimate about printing ink discharge characteristic with heterogeneity with 230nm thickness.Its result has been shown in the table 2.
(comparative example 1 to 3)
Use with the example similar methods and estimate printing ink discharge characteristic.Example is estimated the Ta film, the Ta that all have 230nm thickness as a comparison
40Cr
60Film and Ta
28Fe
52Cr
15Ni
5Film.The result has been shown in table 2.
(table 2)
| Film component (at.%) | Crystal structure | Jet velocity | The fouling product | |
| Example 1 | Ta 78Cr 22 | Amorphous state | Well | The pettiness amount |
| Example 2 | Ta 74Cr 26 | Amorphous state | Well | The pettiness amount |
| Example 3 | Ta 70Cr 30 | Amorphous state | Well | The pettiness amount |
| Comparative example 1 | Ta | Crystal | Well | On a small quantity |
| Comparative example 2 | Ta 40Cr 60 | Amorphous state | Bad, not bad | In a large number |
| Comparative example 3 | Ta 28Fe 52Cr 15Ni 5 | Amorphous state | Difference | In a large number |
As shown in table 2, in the Ta film of the TaCr film of example 1 to 3 and comparative example 1, applying 1 * 10
8Kept the velocity of discharge after the driving signal of pulse.On the contrary, in comparative example 2 and 3, the velocity of discharge has reduced, and therefore can not keep the document image of expecting.This spray characteristic is estimated employed ink gun take generation apart with the fouling product of observing its heat action part office.In result's comparative example 2 and 3 that the velocity of discharge reduces greatly therein, observe a large amount of fouling products and be deposited on the heat effect part.Therefore, can confirm the deposition that reduces to cause the fouling product on the ink gun velocity of discharge.This has illustrated that the deposition of fouling product has just become obviously because Ta content has reduced, and this has stoped the maintenance of discharging characteristic.
(example 4)
Use the ink gun similar to carry out the discharge durability test with example 1.In this test, when the pulse width sustained firing by being made as 1 μ sec under the driving frequency at 5kHz detects its service life when ink jet print head can not ink-jet.At this moment, driving voltage V
OpBe V
Th* 1.15.In addition, use comprise about 4% have a nitric acid group divalent metal (Ca (NO
3)
24H
2O) printing ink.Its result has been shown in table 3.
As shown in table 3, even ought be applied to up to 1.0 * 10 continuously by the driving signal
9Pulse is so that during continuous injection printing ink, also can guarantee stable injection.
(example 5 and 6)
Remove respectively with Ta
74Cr
26Film (in the example 5) and Ta
70Cr
30Film (in the example 6) forms outside the upper protective layer 107, to prepare ink gun with example 4 similar methods.Use these ink guns to spray acceptance test to carry out with example 4 similar methods.Its result has been shown in table 3.
(comparative example 4 and 5)
Remove respectively with Ta film (in the comparative example 4) and Ta
89Cr
11Film (in the comparative example 5) forms outside the upper protective layer 107, to prepare ink gun with example 4 similar methods.Use these ink guns to spray acceptance test to carry out with example 4 similar methods.Its result has been shown in table 3.
As shown in table 3, in comparative example 4 and 5, apply 4 * 10 in arrival
8Damage occurred before the driving signal of pulse, thereby can not spray.
The above results has illustrated following situation.Shown in the result in the table 3, we find to discharge the durability shown in the durability test obviously depends on its crystal structure and changes into amorphous structure and will increase durability.
Table 3
| Film component (at.%) | Crystal structure | The number of pulses of normal injection | |
| Example 4 | Ta 78Cr 22 | Amorphous state | 1.0×10 9Pulse or bigger |
| Example 5 | Ta 74Cr 26 | Amorphous state | 1.0×10 9Pulse or bigger |
| Example 6 | Ta 70Cr 30 | Amorphous state | 1.0×10 9Pulse or bigger |
| Comparative example 4 | Ta | Crystal | 4.0×10 8Pulse or littler |
| Comparative example 5 | Ta 89Cr 11 | Crystal | 4.0×10 8Pulse or littler |
Discharge durability test up to having applied 1 * 10 for wherein carrying out
9The heating resistor of the ink gun of the example 4 of the driving signal of pulse and wherein carry out to discharge the unspoiled heating resistor of the ink gun of the comparative example 4 that the part of durability test in a plurality of heating resistors damaged is carried out cross-sectional view.At Fig. 6 A their illustrative figure has been shown in the 6C.Here, Fig. 6 A shows the original state of example 4 and comparative example 4, and Reference numeral 401 expressions and upper protective layer 107 corresponding layers wherein are Ta in the example 4
78Cr
22Film, and be the Ta film in the comparative example 4.In addition, Reference numeral 108 expression heat effect parts, Reference numeral 106 expression insulating protective layers, Reference numeral 105 expression metal lines and Reference numeral 104 expression thermoresistance layers.Fig. 6 B carries out to discharge durability afterwards up to 1.0 * 10
9The driving signal of pulse is applied to the illustrative sectional view of heating resistor of the ink gun of example 4, and Reference numeral 402 expressions are formed on the oxide-film on the upper protective layer 107.Fig. 6 C is when arriving 4 * 10
8The illustrative sectional view of the unspoiled heating resistor when the part heating resistor of the ink gun of comparative example 4 was damaged before the driving signal of pulse was applied in, and Reference numeral 403 expressions are formed on the oxide-film on the upper protective layer 107.
From these results, in comparative example 4, it is oxidized and have a local zone of getting deeply stuck in oxide-film that we observe most of Ta on the heat effect part as shown in oxide-film 403.Can infer that this etch state has reached thermoresistance layer 104 in the heating resistor of the damage of comparative example 4, this has caused damage.
On the contrary, in example 4, on the upper protective layer on the heat effect part 108 107 (401), be formed with oxide layer 402 as thin as a wafer.Its thickness is approximately 10nm.Although whole film thickness is reduced to about 190nm slightly, most of film remains on metallic state.As a result, can infer, irrelevant by wherein being formed with a kind of like this structure of oxide-film 402 with the generation of fouling product, when keeping durability, can keep good discharge characteristic.
Aforesaid; according to example 1 to 6; on the upper protective layer that has with the printing ink contact surface, produce in the ink gun of fouling product therein by the driving of heating resistor; by forming the upper protective layer of making by the amorphous alloy that comprises Ta and Cr (wherein the content of Ta is greater than the content of Cr); can be provided at the outstanding ink gun of cavitation resistance and corrosion resistance aspect; and have high durability, have the similar discharging performance of making to the Ta film of traditional protection layer simultaneously.
(2) structure of upper protective layer and the relation between the etching
Next, will be described in below that the employed upper protective layer that is used for the substrate of ink-jet in the above-mentioned test is formed and form this fact that the present invention was suitable under the situation of pattern upper protective layer is brought specific action by dry etching.
At first, prepare such sample, wherein on forming the metal film of the related film of example 1 to 8, the above-mentioned film of the use with corresponding composition forms photoresist with reservation shape, and under the power of 300W, carry out dry etching, use reactive ion etch equipment flow with 100sccm under the pressure of 1Pa to introduce Cl simultaneously for each sample
2Gas.Figure 7 illustrates its result.
Illustrated among Fig. 7 and used Cl
2Gas is carried out under the situation of dry etching, and etching speed depends on the Ta amount and reduces along with the minimizing of Ta amount.
In this test, although use Cl
2Gas is carried out dry etching.But be to use Cl
2The mist of gas and other gases or use the situation of other gases also to demonstrate similar trend.
(example 7)
After upper protective layer 107 stands dry etching, carry out reliability testing for the reliability of estimating protective layer.
Fig. 8 A is the illustrative sectional view that is used for the substrate of ink-jet to 8E.Here, Reference numeral 106 expression insulating protective layers, Reference numeral 107 expression upper protective layer, Reference numeral 521 expressions comprise the heater substrate of silicon substrate 101, heat accumulation layer 102, interlayer film 103, thermoresistance layer 104 and metal wiring layer 105.Reference numeral 522 shows the heat part 108 that is formed by thermoresistance layer 104 and the metal line 105 with the structure shown in Fig. 1 abstractively.In addition, Reference numeral 523 expression resists.
In this test, estimates whether insufficient by the insulating protective layer covering by etching away insulating protective layer (the part B among Fig. 8 E) below the upper protective layer.In order to make this evaluation, in BHF (hydrofluoric acid that contains buffer) solution, soak the substrate 20 minutes that is used for ink-jet, and in 3% NaOH (NaOH) solution, soak the substrate 10 minutes that is used for ink-jet.Set etching condition according to predefined etching speed, so that can carry out 20% over etching.About example 7, can be observed etch state and whether develop from the etched part of insulating protective layer (the part B among Fig. 8 E).As a result, never find in the fact of the part that etch state develops.Can confirm to have kept the reliability of protective layer.
(example 8 to 12)
To carry out reliability testing with respect to TaCr film with heterogeneity with example 7 similar methods.Its result has been shown in table 4.
(comparative example 6 to 9)
To carry out reliability testing with example 7 similar methods.Example is estimated Ta film, Ta as a comparison
40Cr
60Film, Ta
28Fe
52Cr
15Ni
5Film and Ta
17Fe
54Cr
25Ni
4, its result has been shown in table 4.
(table 4)
| Film component (at.%) | Insulating protective layer | Film thickness [nm] | Soak Test in BHF and 3% NaOH solution | |
| Example 7 | Ta 78Cr 22 | SiN | 230 | Well |
| Example 8 | Ta 89Cr 11 | SiN | 230 | Well |
| Example 9 | Ta 74Cr 26 | SiN | 230 | Well |
| Example 10 | Ta 70Cr 30 | SiN | 230 | Well |
| Example 11 | Ta 55Cr 45 | SiN | 230 | Bad, not bad |
| Example 12 | Ta 55Cr 45 | SiN | 150 | Well |
| Comparative example 6 | Ta | SiN | 230 | Well |
| Comparative example 7 | Ta 40Cr 60 | SiN | 230 | Difference |
| Comparative example 8 | Ta 28Fe 52Cr 15Ni 5 | SiN | 230 | Difference |
| Comparative example 9 | Ta 17Fe 54Cr 25Ni 4 | SiN | 230 | Difference |
As shown in table 4, in comparative example 7 to 9,, in the part B of Fig. 8 E, observe certain corrosion of wiring layer because insulating protective layer has been corroded in etching.On the contrary, in example 7 to 10 and comparative example 6, do not observe corrosion, this explanation has kept the reliability of insulating protective layer.And; in example 11, because macro-corrosion is observed in the reduction of etching speed, and film thickness in the situation of thin example 12 therein; the etch quantity of insulating protective layer has reduced because therefore etching period has reduced, and does not observe corrosion in reliability testing.
These presentation of results, owing to the minimizing of etching speed along with Ta content reduces, so etching reaches protective layer deeply, this make cover insufficient.
(example 13 to 15)
Except that SiO as the protective layer 106, use with example 9 to 11 in the similar substrate execution reliability testing similar that is used for ink-jet to table 3.The result has been shown in table 5.
(comparative example 10)
Remove Ta
17Fe
54Cr
25Ni
4As outside the upper protective layer, use with example 13 to 15 in the similar substrate execution reliability testing similar that is used for ink-jet to table 4.The result has been shown in table 5.
(table 5)
| Film component (at.%) | Insulating protective layer | Film thickness [nm] | Soak Test in BHF and 3% NaOH solution | |
| Example 13 | Ta 74Cr 26 | SiO | 230 | Well |
| Example 14 | Ta 70Cr 30 | SiO | 230 | Well |
| Example 15 | Ta 55Cr 45 | SiO | 230 | Well |
| Comparative example 10 | Ta 17Fe 54Cr 25Ni 4 | SiO | 230 | Difference |
As shown in table 5, in example 13 to 15, do not observe corrosion.This is because make the therefore covering that has kept protective layer because the etching speed of SiO is lower than etching speed and the protective layer 106 usefulness SiO of SiN.On the contrary, in comparative example 10, observed certain corrosion.
Although even in zone with low Ta content by making TaCr thinner or by optionally base material being changed into the reliability that suitable material also can keep insulating protective layer; but for the durability that reaches insulating protective layer and the balance between the reliability, the content of Cr is preferably 30at.% or lower.
Aforesaid; according to above-mentioned example 7 to 15; be used for having the insulating protective layer that is located on the heating resistor and be formed on the upper protective layer on the insulating protective layer and form the substrate of the ink gun of pattern by dry etching; by forming the upper protective layer of making by the alloy that comprises Ta and Cr (wherein the content of Ta is greater than the content of Cr); even by dry etching is that upper protective layer forms pattern, can avoid reducing protective capability with the contacted insulating protective layer of upper protective layer.Therefore, provide to have outstanding protective layer aspect cavitation resistance and corrosion resistance, and have high durability.Particularly, by comprising ink gun, can realize higher cavitation resistance, corrosion resistance and durability in conjunction with the structure described in the example 1 to 15.
Claims (6)
1. substrate that is used for ink gun comprises:
Heating resistor produces the heat energy that is used to spray printing ink;
Be located at the insulating protective layer of described heating resistor top; And
Upper protective layer, described upper protective layer is formed on the top of described insulating protective layer, has the contact surface that contacts with printing ink,
Wherein, described upper protective layer is made by the amorphous alloy that Ta and Cr form, and wherein the content of Cr is smaller or equal to 30at.%.
2. according to the described substrate that is used for ink gun of claim 1, it is characterized in that the thickness of upper protective layer is smaller or equal to 500nm more than or equal to 50nm.
3. according to claim 1 or the 2 described substrates that are used for ink gun, it is characterized in that upper protective layer has smaller or equal to 1.0 * 10
10Dyn/cm
2Compression stress.
4. ink gun comprises:
The printing ink ejiction opening; And
Substrate; This substrate comprises: heating resistor is used to produce the heat energy from described printing ink ejiction opening ejection printing ink;
Be located at the insulating protective layer of described heating resistor top; And
Upper protective layer, described upper protective layer is formed on the top of described insulating protective layer, has the contact surface that contacts with printing ink,
Wherein, described upper protective layer is made by the amorphous alloy that Ta and Cr form, and wherein the content of Cr is smaller or equal to 30at.%.
5. manufacture method that is used for the substrate of ink gun comprises:
Order forms the step of heating resistor and insulating protective layer on the described substrate that is used for ink gun,
Wherein, above described insulating protective layer, form the upper protective layer of content that the amorphous alloy is made up of Ta and Cr is made, wherein Cr smaller or equal to 30at.%, and by dry etching to described upper protective layer formation pattern.
6. according to the described manufacture method that is used for the ink gun substrate of claim 5, it is characterized in that, upper protective layer is formed pattern by the dry etching that uses chlorine.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP380821/2002 | 2002-12-27 | ||
| JP380875/2002 | 2002-12-27 | ||
| JP2002380821 | 2002-12-27 | ||
| JP413499/2003 | 2003-12-11 |
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| Publication Number | Publication Date |
|---|---|
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| CN100496979C true CN100496979C (en) | 2009-06-10 |
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ID=35964218
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|---|---|---|---|
| CNB2003801075185A Expired - Fee Related CN100496979C (en) | 2002-12-27 | 2003-12-25 | Substrate for ink jet head, ink jet head using the same, and manufacturing method thereof |
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| JP6150519B2 (en) | 2012-12-27 | 2017-06-21 | キヤノン株式会社 | INKJET RECORDING HEAD SUBSTRATE, INKJET RECORDING HEAD, INKJET RECORDING HEAD MANUFACTURING METHOD, INKJET RECORDING DEVICE, AND INKJET RECORDING HEAD SUBSTRATE |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1348865A (en) * | 2000-09-04 | 2002-05-15 | 佳能株式会社 | Recording device and image recording apparatus |
| US6485131B1 (en) * | 1999-10-04 | 2002-11-26 | Canon Kabushiki Kaisha | Ink-jet head base board, ink-jet head, and ink-jet apparatus |
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2003
- 2003-12-25 CN CNB2003801075185A patent/CN100496979C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6485131B1 (en) * | 1999-10-04 | 2002-11-26 | Canon Kabushiki Kaisha | Ink-jet head base board, ink-jet head, and ink-jet apparatus |
| CN1348865A (en) * | 2000-09-04 | 2002-05-15 | 佳能株式会社 | Recording device and image recording apparatus |
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