Hard x-ray nanoimaging enables structural investigations of new materials for many applications. For high-resolution experiments, zone plate x-ray optics are commonly chosen.Two methods of zone plate nanofabrication are presented in this thesis.

Zone plates are circular diffraction gratings with radially decreasing grating period. Their optical resolution depends on the width of the smallest zone, which nowadays can be around 10 nanometers. However, the efficiency of a zone plate depends on its thickness and its material. For hard x-rays, the optimal zone plate thickness is in the order of micrometers. Therefore, high aspect ratio nanofabrication processes are needed.Two such methods are investigated in this study.

First, an existing tungsten nanofabrication process based on reactive ion etching (RIE) was extended to 22:1 aspect ratio structures at 30~nm line width. The core improvement was a resist curing step that enhanced pattern transfer during RIE. Such a zone plate with 200 micrometer diameter and 2.2% efficiency was used in the commissioning experiment of NanoMAX, the nanoimaging beamline at the Swedish synchrotron facility MAX IV. Transmission imaging with 40 nm resolution, as well as the fluorescence imaging modality were demonstrated.

Second, metal-assisted chemical etching (MACE) of silicon using gold catalyst patterns was investigated. MACE dependence on gold pattern geometry, etching solution composition, temperature, and substrate doping is described. The process is characterized in terms of etching rate, directionality, and nanostructure surface roughness.

Finally, the Ronchi test is presented as a way to quickly judge the performance of x-ray optics in terms of present aberrations and x-ray sources in terms of coherence.

Hard X-ray scanning microscopes, or nanoprobes, make it possible to image samples and probe their chemical, elemental and structural properties at nanoscale resolution. This is enabled by the use of nanofocusing optics. Commonly used optics in nanoprobes for high resolution X-ray experiments are zone plates. Zone plates are circular diffraction optics with radially decreasing grating periods. Their performance depends on their geometrical properties and material. The width of the outermost zone, which today is in the order of a few tens of nanometers, defines the zone plate resolution, while the zone thickness and the material define the X-ray focusing efficiency. For hard X-ray zone plates, the required zone thickness is several micrometers. Therefore, high-aspect ratio nanostructures are a prerequisite for high-resolution, high-efficiency zone plates. The very small structures together with the high-aspect ratios make zone plates one of the most challenging devices to fabricate. A wet-chemical nanofabrication process that has proved its capability of providing silicon nanostructures with ultra-high aspect ratios is metal-assisted chemical etching (MACE). MACE is an electroless, autocatalytic pattern transfer method that uses an etching solution to selectively etch a predefined noble metal pattern into silicon. In this thesis, MACE is optimized specifically for zone plate nanostructures and used in the development of a new zone plate device nanofabrication process. The MACE optimization for silicon zone plate nanostructures involved a systematic investigation of a wide parameter space. The preferable etching solution composition, process temperature, zone plate catalyst design and silicon type were identified. Parameter dependencies were characterized with respect to etching depth and verticality, mechanical stability of zones and silicon surface roughness. Zone plate molds with aspect ratios of 30:1 at 30 nm zone widths were nanofabricated using the optimized MACE process. For use with hard X-rays, the silicon molds were metallized with palladium using electroless deposition (ELD). The first order diffraction efficiency of such a palladium/silicon zone plate was characterized as 1.9 %. Both MACE for the zone plate pattern transfer and ELD for the silicon mold metalization are conceptually simple, relatively low-cost and accessible methods, which opens up for further developments of zone plate device nanofabrication processes.

Hårdröntgensvepmikroskopi möjliggör avbildandet av prover och karaktärisering av dem kemiska, elementära och strukturella egenskaperna med nanometerupplösning. Detta är tack vare användandet av nanofokuserande optik. Vanligen förekommande optik i röntgenmikroskop för högupplösta analyser är zonplattor. Zonplattor är cirkulära diffraktionsoptik med radiellt avtagande gitterperiod. Deras prestanda beror på de geometriska egenskaperna och materialet de är gjorda av. Bredden på den yttersta zonen, vilken vanligtvis är i storleksordningen av några tiotal nanometer, definierar zonplattans optiska upplösning medan zontjockleken samt dess material definierar verkningsgraden. För hårdröntgenzonplattor krävs ofta en zontjocklek på några mikrometer. Detta gör nanostrukturer med stort tjocklek-breddförhållande en förutsättning för högupplösta zonplattor med hög verkningsgrad. De väldigt små strukturerna och det stora tjocklek-breddförhållandet gör zonplattor utmanande att tillverka. En våtkemisk nanofabrikationsprocess som har påvisat sin förmåga att tillverka kiselnanostrukturer med extrema tjocklek-breddförhållanden är metall-assisterad kemisk etsning (MACE). MACE är en elektrofri, autokatalytisk process där fördefinierade ädelmetallstrukturer med hjälp av en etslösning selektivt etsar kisel. I denna avhandling optimeras MACE specifikt för nanometerstora zonplattestrukturer och används i en ny nanofabrikationsprocess utvecklad för framtagning av zonplattor. Optimeringen av MACE för zonplattestrukturer i kisel utgjordes av en systematisk och omfattande parameterstudie. Den bättre kompositionen av etslösningen, processtemperaturen, zonplattedesignen och kiselsubstratet identifierades. Processen karaktäriserades med avseende på zonplattans tjocklek och etsriktningen, den mekaniska stabiliteten av zoner och ytråheten hos kislet. Kiselzonplattor med ett tjocklek-breddförhållande på 30:1 med en minsta zonbredd på 30 nm tillverkades med den optimerade MACE processen. Inför användning med hårdröntgen metalliserades kiselzonplattorna med palladium via en autokatalytisk pläteringsprocess (ELD). Verkningsgraden av första ordningens diffraktion för en sådan palladium/kiselzonplatta karaktäriserades till 1.9 %. Både MACE och ELD är konceptuellt enkla, relativt låga i kostnad och tillgängliga metoder som kommer bana väg för det vidare utvecklandet av nanofabrikationsprocesser för zonplatteframställning.